# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2004133'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-14 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
bis(μ2-sulfido)-bis(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-diniobium(V)
_chemical_name_common            '[(BDI)Nb(NtBu)(μ-S)]2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H100 N6 Nb2 S2'
_chemical_formula_sum            'C66 H100 N6 Nb2 S2'
_chemical_formula_weight         1227.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.292(5)
_cell_length_b                   14.181(5)
_cell_length_c                   22.910(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 117.461(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     6426(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9809
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      25.36

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_F_000             2608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.465
_shelx_estimated_absorpt_T_min   0.737
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7023
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            70667
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.767
_diffrn_reflns_theta_max         25.380
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5882
_reflns_number_gt                5565
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR-97
_computing_structure_refinement  SHELXL-2014
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0248P)²+13.4028P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5882
_refine_ls_number_parameters     356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0228
_refine_ls_wR_factor_ref         0.0598
_refine_ls_wR_factor_gt          0.0586
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.20368(8) -0.05646(11) 0.03692(8) 0.0159(3) Uani 1 1 d . . . . .
C2 C 0.17116(8) -0.03400(11) 0.07503(8) 0.0150(3) Uani 1 1 d . . . . .
H2 H 0.1406 -0.0803 0.0755 0.018 Uiso 1 1 calc R U . . .
C3 C 0.17738(8) 0.04665(11) 0.11239(8) 0.0133(3) Uani 1 1 d . . . . .
C4 C 0.20204(11) -0.15996(12) 0.02016(11) 0.0275(4) Uani 1 1 d . . . . .
H4A H 0.1736 -0.1689 -0.0272 0.041 Uiso 1 1 calc R U . . .
H4B H 0.1835 -0.1963 0.0445 0.041 Uiso 1 1 calc R U . . .
H4C H 0.2480 -0.1817 0.0323 0.041 Uiso 1 1 calc R U . . .
C5 C 0.16225(9) 0.03308(12) 0.16981(8) 0.0186(4) Uani 1 1 d . . . . .
H5A H 0.2047 0.0316 0.2109 0.028 Uiso 1 1 calc R U . . .
H5B H 0.1380 -0.0265 0.1645 0.028 Uiso 1 1 calc R U . . .
H5C H 0.1342 0.0854 0.1712 0.028 Uiso 1 1 calc R U . . .
C6 C 0.27985(9) -0.03328(11) -0.00760(8) 0.0149(3) Uani 1 1 d . . . . .
C7 C 0.25272(9) -0.05662(12) -0.07448(9) 0.0187(4) Uani 1 1 d . . . . .
C8 C 0.29573(10) -0.09777(12) -0.09653(10) 0.0243(4) Uani 1 1 d . . . . .
H8 H 0.2783 -0.1143 -0.1416 0.029 Uiso 1 1 calc R U . . .
C9 C 0.36285(10) -0.11477(13) -0.05421(10) 0.0268(4) Uani 1 1 d . . . . .
H9 H 0.3910 -0.1439 -0.0699 0.032 Uiso 1 1 calc R U . . .
C10 C 0.38891(10) -0.08937(13) 0.01092(10) 0.0240(4) Uani 1 1 d . . . . .
H10 H 0.4354 -0.1004 0.0397 0.029 Uiso 1 1 calc R U . . .
C11 C 0.34849(9) -0.04780(12) 0.03563(9) 0.0186(4) Uani 1 1 d . . . . .
C12 C 0.17956(10) -0.03847(13) -0.12446(9) 0.0240(4) Uani 1 1 d . . . . .
H12 H 0.1552 -0.0128 -0.1005 0.029 Uiso 1 1 calc R U . . .
C13 C 0.14342(12) -0.12898(17) -0.16025(12) 0.0423(6) Uani 1 1 d . . . . .
H13A H 0.1656 -0.1541 -0.1852 0.063 Uiso 1 1 calc R U . . .
H13B H 0.0960 -0.1147 -0.1904 0.063 Uiso 1 1 calc R U . . .
H13C H 0.1455 -0.1759 -0.1279 0.063 Uiso 1 1 calc R U . . .
C14 C 0.17551(11) 0.03457(15) -0.17516(9) 0.0317(5) Uani 1 1 d . . . . .
H14A H 0.1919 0.0955 -0.1534 0.048 Uiso 1 1 calc R U . . .
H14B H 0.1285 0.0409 -0.2091 0.048 Uiso 1 1 calc R U . . .
H14C H 0.2036 0.0141 -0.1955 0.048 Uiso 1 1 calc R U . . .
C15 C 0.37928(9) -0.01961(13) 0.10751(9) 0.0233(4) Uani 1 1 d . . . . .
H15 H 0.3549 0.0379 0.1106 0.028 Uiso 1 1 calc R U . . .
C16 C 0.37018(12) -0.09650(17) 0.14957(11) 0.0400(5) Uani 1 1 d . . . . .
H16A H 0.3219 -0.1080 0.1340 0.060 Uiso 1 1 calc R U . . .
H16B H 0.3909 -0.0760 0.1956 0.060 Uiso 1 1 calc R U . . .
H16C H 0.3920 -0.1547 0.1460 0.060 Uiso 1 1 calc R U . . .
C17 C 0.45395(10) 0.00510(16) 0.13641(11) 0.0355(5) Uani 1 1 d . . . . .
H17A H 0.4800 -0.0520 0.1395 0.053 Uiso 1 1 calc R U . . .
H17B H 0.4694 0.0321 0.1804 0.053 Uiso 1 1 calc R U . . .
H17C H 0.4605 0.0511 0.1080 0.053 Uiso 1 1 calc R U . . .
C18 C 0.21360(8) 0.19926(11) 0.15477(8) 0.0140(3) Uani 1 1 d . . . . .
C19 C 0.27691(9) 0.19897(12) 0.21070(8) 0.0166(3) Uani 1 1 d . . . . .
C20 C 0.28740(9) 0.25961(13) 0.26256(9) 0.0212(4) Uani 1 1 d . . . . .
H20 H 0.3303 0.2607 0.3004 0.025 Uiso 1 1 calc R U . . .
C21 C 0.23657(10) 0.31798(13) 0.25981(9) 0.0237(4) Uani 1 1 d . . . . .
H21 H 0.2439 0.3569 0.2962 0.028 Uiso 1 1 calc R U . . .
C22 C 0.17518(10) 0.31928(13) 0.20379(9) 0.0223(4) Uani 1 1 d . . . . .
H22 H 0.1407 0.3605 0.2018 0.027 Uiso 1 1 calc R U . . .
C23 C 0.16231(9) 0.26171(12) 0.14980(9) 0.0172(3) Uani 1 1 d . . . . .
C24 C 0.33457(9) 0.13695(13) 0.21559(9) 0.0195(4) Uani 1 1 d . . . . .
H24 H 0.3155 0.0906 0.1786 0.023 Uiso 1 1 calc R U . . .
C25 C 0.38655(10) 0.19680(15) 0.20651(10) 0.0286(4) Uani 1 1 d . . . . .
H25A H 0.3651 0.2266 0.1630 0.043 Uiso 1 1 calc R U . . .
H25B H 0.4239 0.1566 0.2101 0.043 Uiso 1 1 calc R U . . .
H25C H 0.4041 0.2456 0.2406 0.043 Uiso 1 1 calc R U . . .
C26 C 0.36748(10) 0.08097(14) 0.27984(10) 0.0281(4) Uani 1 1 d . . . . .
H26A H 0.3899 0.1245 0.3169 0.042 Uiso 1 1 calc R U . . .
H26B H 0.4009 0.0373 0.2786 0.042 Uiso 1 1 calc R U . . .
H26C H 0.3327 0.0453 0.2852 0.042 Uiso 1 1 calc R U . . .
C27 C 0.09416(9) 0.26950(12) 0.08894(9) 0.0204(4) Uani 1 1 d . . . . .
H27 H 0.0965 0.2320 0.0531 0.024 Uiso 1 1 calc R U . . .
C28 C 0.03626(10) 0.22922(14) 0.10015(11) 0.0294(4) Uani 1 1 d . . . . .
H28A H 0.0441 0.1619 0.1105 0.044 Uiso 1 1 calc R U . . .
H28B H -0.0067 0.2377 0.0602 0.044 Uiso 1 1 calc R U . . .
H28C H 0.0345 0.2624 0.1369 0.044 Uiso 1 1 calc R U . . .
C29 C 0.07886(10) 0.37223(14) 0.06559(10) 0.0261(4) Uani 1 1 d . . . . .
H29A H 0.0735 0.4099 0.0988 0.039 Uiso 1 1 calc R U . . .
H29B H 0.0371 0.3748 0.0239 0.039 Uiso 1 1 calc R U . . .
H29C H 0.1163 0.3976 0.0592 0.039 Uiso 1 1 calc R U . . .
C30 C 0.04654(8) 0.13573(13) -0.08767(9) 0.0205(4) Uani 1 1 d . . . . .
C31 C 0.01721(10) 0.07670(17) -0.05137(11) 0.0363(5) Uani 1 1 d . . . . .
H31A H 0.0355 0.0126 -0.0452 0.054 Uiso 1 1 calc R U . . .
H31B H -0.0321 0.0745 -0.0772 0.054 Uiso 1 1 calc R U . . .
H31C H 0.0294 0.1051 -0.0084 0.054 Uiso 1 1 calc R U . . .
C32 C 0.02951(10) 0.09264(17) -0.15408(10) 0.0337(5) Uani 1 1 d . . . . .
H32A H 0.0509 0.1296 -0.1755 0.051 Uiso 1 1 calc R U . . .
H32B H -0.0196 0.0929 -0.1816 0.051 Uiso 1 1 calc R U . . .
H32C H 0.0462 0.0276 -0.1480 0.051 Uiso 1 1 calc R U . . .
C33 C 0.01791(10) 0.23673(16) -0.09848(11) 0.0346(5) Uani 1 1 d . . . . .
H33A H 0.0302 0.2663 -0.0558 0.052 Uiso 1 1 calc R U . . .
H33B H -0.0314 0.2345 -0.1242 0.052 Uiso 1 1 calc R U . . .
H33C H 0.0368 0.2736 -0.1223 0.052 Uiso 1 1 calc R U . . .
N1 N 0.23674(7) 0.00579(9) 0.01878(7) 0.0127(3) Uani 1 1 d . . . . .
N2 N 0.20001(6) 0.13001(9) 0.10317(7) 0.0120(3) Uani 1 1 d . . . . .
N3 N 0.11943(7) 0.14151(10) -0.04592(7) 0.0145(3) Uani 1 1 d . . . . .
S1 S 0.22071(2) 0.32032(3) 0.03865(2) 0.01708(10) Uani 1 1 d . . . . .
Nb1 Nb 0.20513(2) 0.15698(2) 0.01084(2) 0.00954(5) Uani 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.333(2) . ?
C1 C2 1.405(2) . ?
C1 C4 1.513(2) . ?
C2 C3 1.397(2) . ?
C2 H2 0.9500 . ?
C3 N2 1.340(2) . ?
C3 C5 1.513(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C11 1.403(2) . ?
C6 C7 1.403(2) . ?
C6 N1 1.460(2) . ?
C7 C8 1.401(2) . ?
C7 C12 1.521(3) . ?
C8 C9 1.378(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.376(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.396(2) . ?
C10 H10 0.9500 . ?
C11 C15 1.517(3) . ?
C12 C14 1.528(3) . ?
C12 C13 1.536(3) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.522(3) . ?
C15 C16 1.529(3) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.402(2) . ?
C18 C23 1.409(2) . ?
C18 N2 1.457(2) . ?
C19 C20 1.396(2) . ?
C19 C24 1.518(2) . ?
C20 C21 1.381(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.379(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.397(2) . ?
C22 H22 0.9500 . ?
C23 C27 1.520(2) . ?
C24 C25 1.526(3) . ?
C24 C26 1.529(3) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C29 1.535(3) . ?
C27 C28 1.538(3) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N3 1.459(2) . ?
C30 C32 1.517(3) . ?
C30 C31 1.524(3) . ?
C30 C33 1.541(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
N1 Nb1 2.2378(15) . ?
N2 Nb1 2.2037(14) . ?
N3 Nb1 1.7599(14) . ?
S1 Nb1 2.3850(9) . ?
S1 Nb1 2.4190(6) 7 ?
Nb1 S1 2.4191(6) 7 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 124.16(15) . . ?
N1 C1 C4 121.02(15) . . ?
C2 C1 C4 114.75(15) . . ?
C3 C2 C1 129.26(15) . . ?
C3 C2 H2 115.4 . . ?
C1 C2 H2 115.4 . . ?
N2 C3 C2 124.34(15) . . ?
N2 C3 C5 120.02(14) . . ?
C2 C3 C5 115.44(14) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 121.13(15) . . ?
C11 C6 N1 118.39(15) . . ?
C7 C6 N1 120.47(15) . . ?
C8 C7 C6 118.05(17) . . ?
C8 C7 C12 118.26(16) . . ?
C6 C7 C12 123.68(15) . . ?
C9 C8 C7 121.40(18) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C10 C9 C8 119.69(17) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C9 C10 C11 121.43(18) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C10 C11 C6 118.26(17) . . ?
C10 C11 C15 119.86(16) . . ?
C6 C11 C15 121.87(15) . . ?
C7 C12 C14 110.73(16) . . ?
C7 C12 C13 112.13(16) . . ?
C14 C12 C13 109.15(17) . . ?
C7 C12 H12 108.2 . . ?
C14 C12 H12 108.2 . . ?
C13 C12 H12 108.2 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C17 112.93(16) . . ?
C11 C15 C16 111.79(16) . . ?
C17 C15 C16 109.05(17) . . ?
C11 C15 H15 107.6 . . ?
C17 C15 H15 107.6 . . ?
C16 C15 H15 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 120.87(15) . . ?
C19 C18 N2 118.98(14) . . ?
C23 C18 N2 120.05(14) . . ?
C20 C19 C18 118.62(16) . . ?
C20 C19 C24 119.34(16) . . ?
C18 C19 C24 122.02(15) . . ?
C21 C20 C19 121.22(17) . . ?
C21 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C22 C21 C20 119.46(17) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C21 C22 C23 121.80(17) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C22 C23 C18 117.91(16) . . ?
C22 C23 C27 118.68(16) . . ?
C18 C23 C27 123.40(15) . . ?
C19 C24 C25 109.75(15) . . ?
C19 C24 C26 112.69(15) . . ?
C25 C24 C26 111.25(15) . . ?
C19 C24 H24 107.6 . . ?
C25 C24 H24 107.6 . . ?
C26 C24 H24 107.6 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 C29 110.86(15) . . ?
C23 C27 C28 112.38(15) . . ?
C29 C27 C28 110.00(15) . . ?
C23 C27 H27 107.8 . . ?
C29 C27 H27 107.8 . . ?
C28 C27 H27 107.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C32 111.61(15) . . ?
N3 C30 C31 107.55(15) . . ?
C32 C30 C31 110.75(17) . . ?
N3 C30 C33 107.86(15) . . ?
C32 C30 C33 108.65(16) . . ?
C31 C30 C33 110.38(17) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C1 N1 C6 116.21(13) . . ?
C1 N1 Nb1 117.46(11) . . ?
C6 N1 Nb1 124.94(10) . . ?
C3 N2 C18 114.79(13) . . ?
C3 N2 Nb1 119.63(11) . . ?
C18 N2 Nb1 125.33(10) . . ?
C30 N3 Nb1 173.08(12) . . ?
Nb1 S1 Nb1 92.916(16) . 7 ?
N3 Nb1 N2 99.70(6) . . ?
N3 Nb1 N1 97.73(6) . . ?
N2 Nb1 N1 84.81(5) . . ?
N3 Nb1 S1 107.05(5) . . ?
N2 Nb1 S1 88.73(4) . . ?
N1 Nb1 S1 155.12(4) . . ?
N3 Nb1 S1 114.45(5) . 7 ?
N2 Nb1 S1 145.30(4) . 7 ?
N1 Nb1 S1 84.72(4) . 7 ?
S1 Nb1 S1 87.084(16) . 7 ?

_refine_diff_density_max         0.600
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.053


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Benzene'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2004136'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-14 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'(2,6-diisopropylphenyl)imino-oxido-4-dimethylaminopyridine-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V) benzene solvate'
_chemical_name_common            (BDI)Nb(NAr)(O)(DMAP)
_chemical_melting_point          492
_chemical_formula_moiety         'C48 H68 N5 Nb O, 0.5(C6 H6)'
_chemical_formula_sum            'C51 H71 N5 Nb O'
_chemical_formula_weight         863.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6646(8)
_cell_length_b                   12.6365(7)
_cell_length_c                   17.2467(10)
_cell_angle_alpha                81.664(2)
_cell_angle_beta                 85.819(3)
_cell_angle_gamma                68.744(2)
_cell_volume                     2343.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9883
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      25.44

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_F_000             922
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.298
_shelx_estimated_absorpt_T_min   0.954
_shelx_estimated_absorpt_T_max   0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7049
_exptl_absorpt_correction_T_max  0.7452






_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            31429
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.194
_diffrn_reflns_theta_max         25.469
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             8583
_reflns_number_gt                7993
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXT
_computing_structure_refinement  SHELXL-2014
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0211P)²+1.8827P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8583
_refine_ls_number_parameters     539
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0732
_refine_ls_wR_factor_gt          0.0716
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.69507(15) 0.74379(14) 0.16978(10) 0.0152(3) Uani 1 1 d . . . . .
C2 C 0.62304(16) 0.74288(15) 0.10793(10) 0.0165(4) Uani 1 1 d . . . . .
H2 H 0.6388 0.7799 0.0585 0.020 Uiso 1 1 calc R U . . .
C3 C 0.53226(15) 0.69555(14) 0.10879(10) 0.0151(3) Uani 1 1 d . . . . .
C4 C 0.81199(16) 0.76538(16) 0.14308(10) 0.0197(4) Uani 1 1 d . . . . .
H4A H 0.8631 0.7535 0.1885 0.030 Uiso 1 1 calc R U . . .
H4B H 0.7912 0.8443 0.1176 0.030 Uiso 1 1 calc R U . . .
H4C H 0.8574 0.7123 0.1058 0.030 Uiso 1 1 calc R U . . .
C5 C 0.49688(17) 0.67820(17) 0.03040(10) 0.0213(4) Uani 1 1 d . . . . .
H5A H 0.5241 0.5961 0.0265 0.032 Uiso 1 1 calc R U . . .
H5B H 0.5363 0.7148 -0.0117 0.032 Uiso 1 1 calc R U . . .
H5C H 0.4073 0.7125 0.0255 0.032 Uiso 1 1 calc R U . . .
C6 C 0.75211(15) 0.72727(14) 0.30166(9) 0.0139(3) Uani 1 1 d . . . . .
C7 C 0.75637(16) 0.83346(15) 0.31439(10) 0.0165(4) Uani 1 1 d . . . . .
C8 C 0.83244(16) 0.83415(16) 0.37306(10) 0.0197(4) Uani 1 1 d . . . . .
H8 H 0.8380 0.9047 0.3817 0.024 Uiso 1 1 calc R U . . .
C9 C 0.89945(17) 0.73514(16) 0.41856(10) 0.0210(4) Uani 1 1 d . . . . .
H9 H 0.9484 0.7380 0.4593 0.025 Uiso 1 1 calc R U . . .
C10 C 0.89558(16) 0.63115(15) 0.40504(10) 0.0191(4) Uani 1 1 d . . . . .
H10 H 0.9426 0.5631 0.4366 0.023 Uiso 1 1 calc R U . . .
C11 C 0.82397(15) 0.62467(15) 0.34610(10) 0.0157(3) Uani 1 1 d . . . . .
C12 C 0.68491(17) 0.94716(15) 0.26619(11) 0.0200(4) Uani 1 1 d . . . . .
H12 H 0.6463 0.9301 0.2220 0.024 Uiso 1 1 calc R U . . .
C13 C 0.77115(19) 1.01001(17) 0.23088(12) 0.0294(5) Uani 1 1 d . . . . .
H13A H 0.8023 1.0361 0.2729 0.044 Uiso 1 1 calc R U . . .
H13B H 0.7258 1.0762 0.1939 0.044 Uiso 1 1 calc R U . . .
H13C H 0.8403 0.9578 0.2034 0.044 Uiso 1 1 calc R U . . .
C14 C 0.58193(18) 1.02655(16) 0.31404(11) 0.0241(4) Uani 1 1 d . . . . .
H14A H 0.5153 0.9962 0.3246 0.036 Uiso 1 1 calc R U . . .
H14B H 0.5502 1.1032 0.2843 0.036 Uiso 1 1 calc R U . . .
H14C H 0.6145 1.0311 0.3638 0.036 Uiso 1 1 calc R U . . .
C15 C 0.82528(16) 0.50988(15) 0.32793(10) 0.0179(4) Uani 1 1 d . . . . .
H15 H 0.7380 0.5173 0.3217 0.021 Uiso 1 1 calc R U . . .
C16 C 0.89442(17) 0.47957(16) 0.25012(10) 0.0218(4) Uani 1 1 d . . . . .
H16A H 0.8521 0.5373 0.2072 0.033 Uiso 1 1 calc R U . . .
H16B H 0.8966 0.4042 0.2407 0.033 Uiso 1 1 calc R U . . .
H16C H 0.9787 0.4779 0.2529 0.033 Uiso 1 1 calc R U . . .
C17 C 0.88069(18) 0.41048(16) 0.39282(11) 0.0240(4) Uani 1 1 d . . . . .
H17A H 0.9685 0.3964 0.3969 0.036 Uiso 1 1 calc R U . . .
H17B H 0.8704 0.3414 0.3801 0.036 Uiso 1 1 calc R U . . .
H17C H 0.8385 0.4302 0.4429 0.036 Uiso 1 1 calc R U . . .
C18 C 0.41523(16) 0.58464(15) 0.16736(9) 0.0151(3) Uani 1 1 d . . . . .
C19 C 0.48123(16) 0.46636(15) 0.17858(10) 0.0173(4) Uani 1 1 d . . . . .
C20 C 0.42098(17) 0.39177(16) 0.16973(10) 0.0212(4) Uani 1 1 d . . . . .
H20 H 0.4646 0.3115 0.1780 0.025 Uiso 1 1 calc R U . . .
C21 C 0.29892(18) 0.43268(16) 0.14907(11) 0.0227(4) Uani 1 1 d . . . . .
H21 H 0.2597 0.3811 0.1413 0.027 Uiso 1 1 calc R U . . .
C22 C 0.23422(17) 0.54945(16) 0.13978(10) 0.0209(4) Uani 1 1 d . . . . .
H22 H 0.1500 0.5772 0.1264 0.025 Uiso 1 1 calc R U . . .
C23 C 0.28956(16) 0.62759(15) 0.14964(10) 0.0171(4) Uani 1 1 d . . . . .
C24 C 0.61558(16) 0.41637(15) 0.20110(11) 0.0202(4) Uani 1 1 d . . . . .
H24 H 0.6445 0.4814 0.2030 0.024 Uiso 1 1 calc R U . . .
C25 C 0.62921(18) 0.34731(16) 0.28324(11) 0.0257(4) Uani 1 1 d . . . . .
H25A H 0.5786 0.3967 0.3212 0.039 Uiso 1 1 calc R U . . .
H25B H 0.7156 0.3187 0.2982 0.039 Uiso 1 1 calc R U . . .
H25C H 0.6021 0.2825 0.2826 0.039 Uiso 1 1 calc R U . . .
C26 C 0.69528(18) 0.34293(17) 0.14033(12) 0.0267(4) Uani 1 1 d . . . . .
H26A H 0.6672 0.2796 0.1365 0.040 Uiso 1 1 calc R U . . .
H26B H 0.7813 0.3122 0.1563 0.040 Uiso 1 1 calc R U . . .
H26C H 0.6884 0.3900 0.0892 0.040 Uiso 1 1 calc R U . . .
C27 C 0.21086(17) 0.75379(16) 0.14539(11) 0.0215(4) Uani 1 1 d . . . . .
H27 H 0.2671 0.7981 0.1425 0.026 Uiso 1 1 calc R U . . .
C28 C 0.13181(18) 0.77487(17) 0.22081(12) 0.0264(4) Uani 1 1 d . . . . .
H28A H 0.0728 0.7355 0.2235 0.040 Uiso 1 1 calc R U . . .
H28B H 0.0872 0.8572 0.2206 0.040 Uiso 1 1 calc R U . . .
H28C H 0.1850 0.7454 0.2664 0.040 Uiso 1 1 calc R U . . .
C29 C 0.12963(19) 0.79714(18) 0.07295(12) 0.0298(5) Uani 1 1 d . . . . .
H29A H 0.1817 0.7844 0.0254 0.045 Uiso 1 1 calc R U . . .
H29B H 0.0826 0.8792 0.0722 0.045 Uiso 1 1 calc R U . . .
H29C H 0.0728 0.7556 0.0750 0.045 Uiso 1 1 calc R U . . .
C30 C 0.26672(16) 0.95639(14) 0.27072(10) 0.0161(3) Uani 1 1 d . . . . .
C31 C 0.23139(17) 1.02776(15) 0.19823(11) 0.0218(4) Uani 1 1 d . . . . .
C32 C 0.1169(2) 1.11424(17) 0.19386(13) 0.0320(5) Uani 1 1 d . . . . .
H32 H 0.0916 1.1610 0.1454 0.038 Uiso 1 1 calc R U . . .
C33 C 0.03848(19) 1.13395(17) 0.25873(13) 0.0342(5) Uani 1 1 d . . . . .
H33 H -0.0401 1.1932 0.2544 0.041 Uiso 1 1 calc R U . . .
C34 C 0.07482(18) 1.06714(16) 0.32969(12) 0.0273(4) Uani 1 1 d . . . . .
H34 H 0.0213 1.0824 0.3742 0.033 Uiso 1 1 calc R U . . .
C35 C 0.18799(16) 0.97804(15) 0.33741(11) 0.0192(4) Uani 1 1 d . . . . .
C36 C 0.32061(18) 1.01037(16) 0.12863(11) 0.0249(4) Uani 1 1 d . . . . .
H36 H 0.3763 0.9282 0.1353 0.030 Uiso 1 1 calc R U . . .
C37 C 0.4009(2) 1.08268(19) 0.12893(12) 0.0329(5) Uani 1 1 d . . . . .
H37A H 0.3492 1.1640 0.1214 0.049 Uiso 1 1 calc R U . . .
H37B H 0.4626 1.0661 0.0863 0.049 Uiso 1 1 calc R U . . .
H37C H 0.4423 1.0643 0.1792 0.049 Uiso 1 1 calc R U . . .
C38 C 0.2599(2) 1.03464(19) 0.04923(12) 0.0353(5) Uani 1 1 d . . . . .
H38A H 0.2081 0.9884 0.0496 0.053 Uiso 1 1 calc R U . . .
H38B H 0.3236 1.0150 0.0080 0.053 Uiso 1 1 calc R U . . .
H38C H 0.2091 1.1160 0.0392 0.053 Uiso 1 1 calc R U . . .
C39 C 0.22554(17) 0.90459(16) 0.41567(10) 0.0207(4) Uani 1 1 d . . . . .
H39 H 0.3094 0.8467 0.4081 0.025 Uiso 1 1 calc R U . . .
C40 C 0.2345(3) 0.9740(2) 0.47792(14) 0.0461(6) Uani 1 1 d . . . . .
H40A H 0.2939 1.0116 0.4606 0.069 Uiso 1 1 calc R U . . .
H40B H 0.2619 0.9233 0.5269 0.069 Uiso 1 1 calc R U . . .
H40C H 0.1537 1.0321 0.4866 0.069 Uiso 1 1 calc R U . . .
C41 C 0.1399(3) 0.8394(2) 0.44268(13) 0.0476(7) Uani 1 1 d . . . . .
H41A H 0.0566 0.8938 0.4506 0.071 Uiso 1 1 calc R U . . .
H41B H 0.1690 0.7905 0.4921 0.071 Uiso 1 1 calc R U . . .
H41C H 0.1391 0.7918 0.4028 0.071 Uiso 1 1 calc R U . . .
C42 C 0.56423(16) 0.78432(15) 0.44406(10) 0.0173(4) Uani 1 1 d . . . . .
H42 H 0.5380 0.8589 0.4156 0.021 Uiso 1 1 calc R U . . .
C43 C 0.61592(16) 0.76977(15) 0.51501(10) 0.0185(4) Uani 1 1 d . . . . .
H43 H 0.6225 0.8334 0.5352 0.022 Uiso 1 1 calc R U . . .
C44 C 0.65976(16) 0.65950(16) 0.55858(10) 0.0178(4) Uani 1 1 d . . . . .
C45 C 0.63207(16) 0.57348(15) 0.52812(10) 0.0173(4) Uani 1 1 d . . . . .
H45 H 0.6505 0.4997 0.5572 0.021 Uiso 1 1 calc R U . . .
C46 C 0.57878(16) 0.59717(15) 0.45671(10) 0.0161(4) Uani 1 1 d . . . . .
H46 H 0.5624 0.5375 0.4374 0.019 Uiso 1 1 calc R U . . .
C47 C 0.75120(19) 0.72723(17) 0.65465(11) 0.0255(4) Uani 1 1 d . . . . .
H47A H 0.7997 0.7586 0.6155 0.038 Uiso 1 1 calc R U . . .
H47B H 0.7980 0.6955 0.7028 0.038 Uiso 1 1 calc R U . . .
H47C H 0.6739 0.7883 0.6660 0.038 Uiso 1 1 calc R U . . .
C48 C 0.77945(17) 0.51883(16) 0.66086(10) 0.0226(4) Uani 1 1 d . . . . .
H48A H 0.7141 0.4902 0.6815 0.034 Uiso 1 1 calc R U . . .
H48B H 0.8317 0.5156 0.7038 0.034 Uiso 1 1 calc R U . . .
H48C H 0.8294 0.4713 0.6218 0.034 Uiso 1 1 calc R U . . .
C49 C 0.87980(19) 0.51724(18) 0.02382(12) 0.0308(5) Uani 1 1 d . . . . .
H49 H 0.7970 0.5293 0.0402 0.037 Uiso 1 1 calc R U . . .
C50 C 0.97204(19) 0.41432(17) 0.04762(11) 0.0274(4) Uani 1 1 d . . . . .
H50 H 0.9528 0.3554 0.0803 0.033 Uiso 1 1 calc R U . . .
C51 C 1.09177(18) 0.39765(17) 0.02371(11) 0.0260(4) Uani 1 1 d . . . . .
H51 H 1.1553 0.3270 0.0400 0.031 Uiso 1 1 calc R U . . .
N1 N 0.66879(13) 0.72231(12) 0.24541(8) 0.0132(3) Uani 1 1 d . . . . .
N2 N 0.48048(13) 0.66103(12) 0.17482(8) 0.0135(3) Uani 1 1 d . . . . .
N3 N 0.37829(13) 0.86612(12) 0.27455(8) 0.0150(3) Uani 1 1 d . . . . .
N4 N 0.54763(13) 0.70024(12) 0.41142(8) 0.0152(3) Uani 1 1 d . . . . .
N5 N 0.72449(14) 0.63724(13) 0.62425(8) 0.0212(3) Uani 1 1 d . . . . .
O O 0.40224(11) 0.62588(10) 0.32947(7) 0.0178(3) Uani 1 1 d . . . . .
Nb Nb 0.47969(2) 0.71711(2) 0.28903(2) 0.01228(5) Uani 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.330(2) . ?
C1 C2 1.409(2) . ?
C1 C4 1.513(2) . ?
C2 C3 1.391(2) . ?
C2 H2 0.9500 . ?
C3 N2 1.341(2) . ?
C3 C5 1.510(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.410(2) . ?
C6 C11 1.410(2) . ?
C6 N1 1.445(2) . ?
C7 C8 1.397(2) . ?
C7 C12 1.529(2) . ?
C8 C9 1.374(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.391(2) . ?
C10 H10 0.9500 . ?
C11 C15 1.522(2) . ?
C12 C14 1.534(3) . ?
C12 C13 1.537(3) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.535(2) . ?
C15 C16 1.538(2) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.403(2) . ?
C18 C23 1.406(2) . ?
C18 N2 1.453(2) . ?
C19 C20 1.394(3) . ?
C19 C24 1.518(2) . ?
C20 C21 1.381(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.384(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.395(3) . ?
C22 H22 0.9500 . ?
C23 C27 1.519(2) . ?
C24 C26 1.529(3) . ?
C24 C25 1.539(2) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C29 1.535(3) . ?
C27 C28 1.536(3) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N3 1.383(2) . ?
C30 C35 1.413(2) . ?
C30 C31 1.423(2) . ?
C31 C32 1.384(3) . ?
C31 C36 1.517(3) . ?
C32 C33 1.384(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.381(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.390(3) . ?
C34 H34 0.9500 . ?
C35 C39 1.518(2) . ?
C36 C38 1.527(3) . ?
C36 C37 1.528(3) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.513(3) . ?
C39 C41 1.520(3) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 N4 1.350(2) . ?
C42 C43 1.363(2) . ?
C42 H42 0.9500 . ?
C43 C44 1.415(2) . ?
C43 H43 0.9500 . ?
C44 N5 1.345(2) . ?
C44 C45 1.417(3) . ?
C45 C46 1.365(2) . ?
C45 H45 0.9500 . ?
C46 N4 1.357(2) . ?
C46 H46 0.9500 . ?
C47 N5 1.456(2) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 N5 1.462(2) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C51 1.379(3) 2_765 ?
C49 C50 1.383(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.376(3) . ?
C50 H50 0.9500 . ?
C51 C49 1.379(3) 2_765 ?
C51 H51 0.9500 . ?
N1 Nb 2.2988(14) . ?
N2 Nb 2.1862(14) . ?
N3 Nb 1.8163(14) . ?
N4 Nb 2.2627(14) . ?
O Nb 1.7497(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 124.56(16) . . ?
N1 C1 C4 121.39(15) . . ?
C2 C1 C4 113.97(14) . . ?
C3 C2 C1 129.32(15) . . ?
C3 C2 H2 115.3 . . ?
C1 C2 H2 115.3 . . ?
N2 C3 C2 123.43(15) . . ?
N2 C3 C5 119.82(15) . . ?
C2 C3 C5 116.67(15) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 120.92(16) . . ?
C7 C6 N1 120.34(14) . . ?
C11 C6 N1 118.65(15) . . ?
C8 C7 C6 118.02(16) . . ?
C8 C7 C12 118.37(16) . . ?
C6 C7 C12 123.59(15) . . ?
C9 C8 C7 121.50(17) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C8 C9 C10 119.99(17) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 C11 121.13(16) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C6 118.37(16) . . ?
C10 C11 C15 121.26(15) . . ?
C6 C11 C15 120.35(15) . . ?
C7 C12 C14 112.62(15) . . ?
C7 C12 C13 111.11(15) . . ?
C14 C12 C13 109.16(15) . . ?
C7 C12 H12 107.9 . . ?
C14 C12 H12 107.9 . . ?
C13 C12 H12 107.9 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C17 113.78(15) . . ?
C11 C15 C16 111.07(14) . . ?
C17 C15 C16 109.08(14) . . ?
C11 C15 H15 107.6 . . ?
C17 C15 H15 107.6 . . ?
C16 C15 H15 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 120.79(16) . . ?
C19 C18 N2 118.03(15) . . ?
C23 C18 N2 121.18(15) . . ?
C20 C19 C18 118.86(16) . . ?
C20 C19 C24 118.70(16) . . ?
C18 C19 C24 122.44(16) . . ?
C21 C20 C19 121.07(17) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C20 C21 C22 119.44(17) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C21 C22 C23 121.69(17) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C22 C23 C18 118.06(16) . . ?
C22 C23 C27 119.02(16) . . ?
C18 C23 C27 122.82(16) . . ?
C19 C24 C26 111.38(15) . . ?
C19 C24 C25 110.18(15) . . ?
C26 C24 C25 111.14(15) . . ?
C19 C24 H24 108.0 . . ?
C26 C24 H24 108.0 . . ?
C25 C24 H24 108.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 C29 112.68(16) . . ?
C23 C27 C28 109.27(15) . . ?
C29 C27 C28 110.63(16) . . ?
C23 C27 H27 108.0 . . ?
C29 C27 H27 108.0 . . ?
C28 C27 H27 108.0 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C35 120.95(15) . . ?
N3 C30 C31 119.09(15) . . ?
C35 C30 C31 119.96(16) . . ?
C32 C31 C30 118.71(18) . . ?
C32 C31 C36 121.52(17) . . ?
C30 C31 C36 119.74(16) . . ?
C33 C32 C31 121.35(18) . . ?
C33 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C34 C33 C32 119.79(18) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 121.46(19) . . ?
C33 C34 H34 119.3 . . ?
C35 C34 H34 119.3 . . ?
C34 C35 C30 118.66(17) . . ?
C34 C35 C39 120.66(16) . . ?
C30 C35 C39 120.67(16) . . ?
C31 C36 C38 114.48(17) . . ?
C31 C36 C37 110.12(16) . . ?
C38 C36 C37 109.92(16) . . ?
C31 C36 H36 107.3 . . ?
C38 C36 H36 107.3 . . ?
C37 C36 H36 107.3 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C35 111.90(16) . . ?
C40 C39 C41 110.88(18) . . ?
C35 C39 C41 111.72(16) . . ?
C40 C39 H39 107.4 . . ?
C35 C39 H39 107.4 . . ?
C41 C39 H39 107.4 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N4 C42 C43 124.63(16) . . ?
N4 C42 H42 117.7 . . ?
C43 C42 H42 117.7 . . ?
C42 C43 C44 119.74(17) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
N5 C44 C43 122.38(17) . . ?
N5 C44 C45 122.01(16) . . ?
C43 C44 C45 115.61(16) . . ?
C46 C45 C44 119.65(16) . . ?
C46 C45 H45 120.2 . . ?
C44 C45 H45 120.2 . . ?
N4 C46 C45 124.41(17) . . ?
N4 C46 H46 117.8 . . ?
C45 C46 H46 117.8 . . ?
N5 C47 H47A 109.5 . . ?
N5 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N5 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N5 C48 H48A 109.5 . . ?
N5 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
N5 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C51 C49 C50 119.91(19) 2_765 . ?
C51 C49 H49 120.0 2_765 . ?
C50 C49 H49 120.0 . . ?
C51 C50 C49 119.65(19) . . ?
C51 C50 H50 120.2 . . ?
C49 C50 H50 120.2 . . ?
C50 C51 C49 120.44(18) . 2_765 ?
C50 C51 H51 119.8 . . ?
C49 C51 H51 119.8 2_765 . ?
C1 N1 C6 117.66(14) . . ?
C1 N1 Nb 122.25(11) . . ?
C6 N1 Nb 118.72(10) . . ?
C3 N2 C18 116.10(14) . . ?
C3 N2 Nb 125.22(11) . . ?
C18 N2 Nb 118.61(10) . . ?
C30 N3 Nb 156.05(12) . . ?
C42 N4 C46 115.37(14) . . ?
C42 N4 Nb 125.55(11) . . ?
C46 N4 Nb 119.04(11) . . ?
C44 N5 C47 120.99(15) . . ?
C44 N5 C48 119.26(15) . . ?
C47 N5 C48 119.45(14) . . ?
O Nb N3 112.39(6) . . ?
O Nb N2 89.24(5) . . ?
N3 Nb N2 102.88(6) . . ?
O Nb N4 86.13(5) . . ?
N3 Nb N4 101.88(6) . . ?
N2 Nb N4 154.70(5) . . ?
O Nb N1 143.72(5) . . ?
N3 Nb N1 103.89(6) . . ?
N2 Nb N1 82.79(5) . . ?
N4 Nb N1 86.32(5) . . ?

_refine_diff_density_max         0.624
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.053
_exptl_special_details           )
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2004134'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-14 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'(N-tert-butylcarbamidato-N,O)-(2,6-diisopropylphenyl)imino-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V) diethyl ether solvate'
_chemical_name_common            (BDI)Nb(NAr)(N(tBu)CO2)
_chemical_melting_point          408
_chemical_formula_moiety         'Nb O2 N4 C46 H67, C4 H10 O'
_chemical_formula_sum            'C50 H77 N4 Nb O3'
_chemical_formula_weight         875.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   18.1386(6)
_cell_length_b                   13.7454(5)
_cell_length_c                   19.8912(7)
_cell_angle_alpha                90
_cell_angle_beta                 106.2880(10)
_cell_angle_gamma                90
_cell_volume                     4760.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9824
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      25.37

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_F_000             1880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.297
_shelx_estimated_absorpt_T_min   0.965
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7071
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            27774
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.888
_diffrn_reflns_theta_max         25.370
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_point_group_measured_fraction_full 0.903
_reflns_number_total             7825
_reflns_number_gt                7465
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.790
_reflns_Friedel_fraction_max     0.791
_reflns_Friedel_fraction_full    0.806

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXT
_computing_structure_refinement  SHELXL-2014
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0360P)²+2.8809P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 3135 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.038(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7825
_refine_ls_number_parameters     542
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0784
_refine_ls_wR_factor_gt          0.0770
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5488(2) 0.5838(3) 0.44298(19) 0.0166(9) Uani 1 1 d . . . . .
C2 C 0.6024(2) 0.6570(3) 0.4647(2) 0.0185(9) Uani 1 1 d . . . . .
H2 H 0.6545 0.6364 0.4789 0.022 Uiso 1 1 calc R U . . .
C3 C 0.5906(2) 0.7576(3) 0.4687(2) 0.0178(9) Uani 1 1 d . . . . .
C4 C 0.5773(2) 0.4859(3) 0.4280(2) 0.0252(10) Uani 1 1 d . . . . .
H4A H 0.5851 0.4443 0.4694 0.038 Uiso 1 1 calc R U . . .
H4B H 0.6260 0.4936 0.4164 0.038 Uiso 1 1 calc R U . . .
H4C H 0.5393 0.4559 0.3884 0.038 Uiso 1 1 calc R U . . .
C5 C 0.6609(2) 0.8199(3) 0.4790(3) 0.0269(10) Uani 1 1 d . . . . .
H5A H 0.6488 0.8761 0.4476 0.040 Uiso 1 1 calc R U . . .
H5B H 0.7019 0.7817 0.4685 0.040 Uiso 1 1 calc R U . . .
H5C H 0.6778 0.8424 0.5277 0.040 Uiso 1 1 calc R U . . .
C6 C 0.4174(2) 0.5230(3) 0.4016(2) 0.0176(8) Uani 1 1 d . . . . .
C7 C 0.4060(2) 0.4436(3) 0.4420(2) 0.0195(10) Uani 1 1 d . . . . .
C8 C 0.3504(3) 0.3743(3) 0.4094(2) 0.0261(10) Uani 1 1 d . . . . .
H8 H 0.3420 0.3192 0.4352 0.031 Uiso 1 1 calc R U . . .
C9 C 0.3081(2) 0.3851(3) 0.3409(2) 0.0279(10) Uani 1 1 d . . . . .
H9 H 0.2701 0.3383 0.3201 0.033 Uiso 1 1 calc R U . . .
C10 C 0.3205(2) 0.4634(3) 0.3019(2) 0.0247(10) Uani 1 1 d . . . . .
H10 H 0.2909 0.4692 0.2544 0.030 Uiso 1 1 calc R U . . .
C11 C 0.3752(2) 0.5341(3) 0.3308(2) 0.0196(9) Uani 1 1 d . . . . .
C12 C 0.4501(3) 0.4294(3) 0.5186(2) 0.0223(10) Uani 1 1 d . . . . .
H12 H 0.4912 0.4802 0.5312 0.027 Uiso 1 1 calc R U . . .
C13 C 0.4887(3) 0.3301(3) 0.5324(3) 0.0331(11) Uani 1 1 d . . . . .
H13A H 0.5214 0.3273 0.5808 0.050 Uiso 1 1 calc R U . . .
H13B H 0.5201 0.3199 0.5002 0.050 Uiso 1 1 calc R U . . .
H13C H 0.4493 0.2793 0.5251 0.050 Uiso 1 1 calc R U . . .
C14 C 0.3978(3) 0.4433(3) 0.5662(2) 0.0282(10) Uani 1 1 d . . . . .
H14A H 0.3539 0.3990 0.5515 0.042 Uiso 1 1 calc R U . . .
H14B H 0.3794 0.5106 0.5627 0.042 Uiso 1 1 calc R U . . .
H14C H 0.4266 0.4291 0.6147 0.042 Uiso 1 1 calc R U . . .
C15 C 0.3901(2) 0.6182(3) 0.2869(2) 0.0230(9) Uani 1 1 d . . . . .
H15 H 0.3978 0.6779 0.3168 0.028 Uiso 1 1 calc R U . . .
C16 C 0.4644(3) 0.6015(4) 0.2659(2) 0.0298(11) Uani 1 1 d . . . . .
H16A H 0.5080 0.5983 0.3081 0.045 Uiso 1 1 calc R U . . .
H16B H 0.4720 0.6553 0.2362 0.045 Uiso 1 1 calc R U . . .
H16C H 0.4606 0.5402 0.2400 0.045 Uiso 1 1 calc R U . . .
C17 C 0.3234(3) 0.6382(4) 0.2222(2) 0.0296(10) Uani 1 1 d . . . . .
H17A H 0.3135 0.5803 0.1923 0.044 Uiso 1 1 calc R U . . .
H17B H 0.3363 0.6931 0.1962 0.044 Uiso 1 1 calc R U . . .
H17C H 0.2774 0.6540 0.2367 0.044 Uiso 1 1 calc R U . . .
C18 C 0.5177(2) 0.9041(3) 0.4515(2) 0.0187(9) Uani 1 1 d . . . . .
C19 C 0.4997(2) 0.9405(3) 0.3825(2) 0.0223(9) Uani 1 1 d . . . . .
C20 C 0.4911(2) 1.0407(3) 0.3741(2) 0.0268(10) Uani 1 1 d . . . . .
H20 H 0.4783 1.0676 0.3283 0.032 Uiso 1 1 calc R U . . .
C21 C 0.5007(3) 1.1017(4) 0.4306(2) 0.0279(11) Uani 1 1 d . . . . .
H21 H 0.4930 1.1697 0.4234 0.033 Uiso 1 1 calc R U . . .
C22 C 0.5214(3) 1.0646(3) 0.4979(2) 0.0270(10) Uani 1 1 d . . . . .
H22 H 0.5298 1.1078 0.5366 0.032 Uiso 1 1 calc R U . . .
C23 C 0.5299(2) 0.9659(3) 0.5096(2) 0.0204(9) Uani 1 1 d . . . . .
C24 C 0.4899(3) 0.8753(3) 0.3191(2) 0.0284(10) Uani 1 1 d . . . . .
H24 H 0.4869 0.8065 0.3345 0.034 Uiso 1 1 calc R U . . .
C25 C 0.4158(3) 0.8980(4) 0.2622(2) 0.0380(12) Uani 1 1 d . . . . .
H25A H 0.3722 0.8951 0.2821 0.057 Uiso 1 1 calc R U . . .
H25B H 0.4086 0.8501 0.2244 0.057 Uiso 1 1 calc R U . . .
H25C H 0.4192 0.9633 0.2435 0.057 Uiso 1 1 calc R U . . .
C26 C 0.5593(3) 0.8837(4) 0.2900(3) 0.0407(14) Uani 1 1 d . . . . .
H26A H 0.5622 0.9499 0.2727 0.061 Uiso 1 1 calc R U . . .
H26B H 0.5538 0.8373 0.2515 0.061 Uiso 1 1 calc R U . . .
H26C H 0.6063 0.8692 0.3272 0.061 Uiso 1 1 calc R U . . .
C27 C 0.5524(2) 0.9279(3) 0.5846(2) 0.0210(9) Uani 1 1 d . . . . .
H27 H 0.5608 0.8562 0.5827 0.025 Uiso 1 1 calc R U . . .
C28 C 0.4878(3) 0.9441(3) 0.6184(2) 0.0265(10) Uani 1 1 d . . . . .
H28A H 0.4800 1.0141 0.6230 0.040 Uiso 1 1 calc R U . . .
H28B H 0.5015 0.9140 0.6650 0.040 Uiso 1 1 calc R U . . .
H28C H 0.4404 0.9148 0.5892 0.040 Uiso 1 1 calc R U . . .
C29 C 0.6271(2) 0.9733(3) 0.6293(2) 0.0316(11) Uani 1 1 d . . . . .
H29A H 0.6686 0.9596 0.6081 0.047 Uiso 1 1 calc R U . . .
H29B H 0.6400 0.9457 0.6766 0.047 Uiso 1 1 calc R U . . .
H29C H 0.6205 1.0439 0.6319 0.047 Uiso 1 1 calc R U . . .
C30 C 0.4539(2) 0.7034(3) 0.6302(2) 0.0163(8) Uani 1 1 d . . . . .
C31 C 0.5274(2) 0.6704(3) 0.6713(2) 0.0179(9) Uani 1 1 d . . . . .
C32 C 0.5437(2) 0.6745(3) 0.7435(2) 0.0224(9) Uani 1 1 d . . . . .
H32 H 0.5927 0.6535 0.7712 0.027 Uiso 1 1 calc R U . . .
C33 C 0.4909(2) 0.7083(3) 0.7768(2) 0.0226(10) Uani 1 1 d . . . . .
H33 H 0.5038 0.7112 0.8264 0.027 Uiso 1 1 calc R U . . .
C34 C 0.4195(2) 0.7377(3) 0.7366(2) 0.0223(9) Uani 1 1 d . . . . .
H34 H 0.3831 0.7604 0.7592 0.027 Uiso 1 1 calc R U . . .
C35 C 0.3993(2) 0.7351(3) 0.6640(2) 0.0184(9) Uani 1 1 d . . . . .
C36 C 0.5870(2) 0.6304(3) 0.6387(2) 0.0217(9) Uani 1 1 d . . . . .
H36 H 0.5651 0.6315 0.5867 0.026 Uiso 1 1 calc R U . . .
C37 C 0.6605(2) 0.6909(4) 0.6579(2) 0.0292(10) Uani 1 1 d . . . . .
H37A H 0.6482 0.7587 0.6440 0.044 Uiso 1 1 calc R U . . .
H37B H 0.6963 0.6652 0.6334 0.044 Uiso 1 1 calc R U . . .
H37C H 0.6842 0.6876 0.7086 0.044 Uiso 1 1 calc R U . . .
C38 C 0.6068(3) 0.5249(3) 0.6616(2) 0.0322(11) Uani 1 1 d . . . . .
H38A H 0.6360 0.5236 0.7112 0.048 Uiso 1 1 calc R U . . .
H38B H 0.6377 0.4963 0.6334 0.048 Uiso 1 1 calc R U . . .
H38C H 0.5593 0.4874 0.6550 0.048 Uiso 1 1 calc R U . . .
C39 C 0.3179(2) 0.7641(3) 0.6227(2) 0.0223(9) Uani 1 1 d . . . . .
H39 H 0.3140 0.7592 0.5717 0.027 Uiso 1 1 calc R U . . .
C40 C 0.2589(3) 0.6935(3) 0.6387(2) 0.0271(10) Uani 1 1 d . . . . .
H40A H 0.2736 0.6264 0.6320 0.041 Uiso 1 1 calc R U . . .
H40B H 0.2079 0.7070 0.6070 0.041 Uiso 1 1 calc R U . . .
H40C H 0.2577 0.7024 0.6873 0.041 Uiso 1 1 calc R U . . .
C41 C 0.2971(3) 0.8685(4) 0.6379(3) 0.0317(12) Uani 1 1 d . . . . .
H41A H 0.3015 0.8753 0.6880 0.048 Uiso 1 1 calc R U . . .
H41B H 0.2442 0.8827 0.6106 0.048 Uiso 1 1 calc R U . . .
H41C H 0.3322 0.9143 0.6249 0.048 Uiso 1 1 calc R U . . .
C42 C 0.2248(2) 0.6749(3) 0.4184(2) 0.0208(9) Uani 1 1 d . . . . .
C43 C 0.2405(3) 0.5872(3) 0.4664(2) 0.0249(10) Uani 1 1 d . . . . .
H43A H 0.2700 0.5390 0.4484 0.037 Uiso 1 1 calc R U . . .
H43B H 0.1917 0.5585 0.4683 0.037 Uiso 1 1 calc R U . . .
H43C H 0.2701 0.6074 0.5135 0.037 Uiso 1 1 calc R U . . .
C44 C 0.1747(2) 0.7487(4) 0.4439(2) 0.0246(9) Uani 1 1 d . . . . .
H44A H 0.2046 0.7772 0.4884 0.037 Uiso 1 1 calc R U . . .
H44B H 0.1295 0.7155 0.4508 0.037 Uiso 1 1 calc R U . . .
H44C H 0.1581 0.8002 0.4089 0.037 Uiso 1 1 calc R U . . .
C45 C 0.1831(2) 0.6423(3) 0.3438(2) 0.0275(10) Uani 1 1 d . . . . .
H45A H 0.1727 0.6990 0.3127 0.041 Uiso 1 1 calc R U . . .
H45B H 0.1345 0.6109 0.3436 0.041 Uiso 1 1 calc R U . . .
H45C H 0.2153 0.5959 0.3274 0.041 Uiso 1 1 calc R U . . .
C46 C 0.3006(3) 0.8085(3) 0.3869(2) 0.0232(9) Uani 1 1 d . . . . .
C47 C 0.7068(7) 0.6355(6) 0.3147(4) 0.121(4) Uani 1 1 d . . . . .
H47A H 0.6617 0.5997 0.3191 0.182 Uiso 1 1 calc R U . . .
H47B H 0.7122 0.6266 0.2674 0.182 Uiso 1 1 calc R U . . .
H47C H 0.7004 0.7049 0.3231 0.182 Uiso 1 1 calc R U . . .
C48 C 0.7736(4) 0.5999(7) 0.3648(6) 0.121(5) Uani 1 1 d . . . . .
H48A H 0.8198 0.6247 0.3532 0.145 Uiso 1 1 calc R U . . .
H48B H 0.7744 0.5280 0.3622 0.145 Uiso 1 1 calc R U . . .
C49 C 0.8210(5) 0.5839(6) 0.4909(6) 0.100(4) Uani 1 1 d . . . . .
H49A H 0.8738 0.5819 0.4860 0.120 Uiso 1 1 calc R U . . .
H49B H 0.8030 0.5158 0.4904 0.120 Uiso 1 1 calc R U . . .
C50 C 0.8241(3) 0.6260(5) 0.5581(4) 0.066(2) Uani 1 1 d . . . . .
H50A H 0.8600 0.6809 0.5673 0.100 Uiso 1 1 calc R U . . .
H50B H 0.8416 0.5768 0.5948 0.100 Uiso 1 1 calc R U . . .
H50C H 0.7728 0.6488 0.5579 0.100 Uiso 1 1 calc R U . . .
N1 N 0.47234(18) 0.5981(2) 0.43300(16) 0.0156(7) Uani 1 1 d . . . . .
N2 N 0.52167(19) 0.7985(2) 0.46117(17) 0.0165(7) Uani 1 1 d . . . . .
N3 N 0.43668(19) 0.7038(2) 0.55723(17) 0.0146(7) Uani 1 1 d . . . . .
N4 N 0.29986(19) 0.7192(2) 0.41955(17) 0.0165(7) Uani 1 1 d . . . . .
O1 O 0.37367(15) 0.8402(2) 0.40731(14) 0.0216(6) Uani 1 1 d . . . . .
O2 O 0.24841(17) 0.8523(2) 0.34761(16) 0.0339(8) Uani 1 1 d . . . . .
O3 O 0.7764(3) 0.6294(3) 0.4358(3) 0.0697(14) Uani 1 1 d . . . . .
Nb Nb 0.41761(2) 0.71703(2) 0.46444(2) 0.01396(10) Uani 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.358(5) . ?
C1 C2 1.381(6) . ?
C1 C4 1.501(6) . ?
C2 C3 1.405(6) . ?
C2 H2 0.9500 . ?
C3 N2 1.340(5) . ?
C3 C5 1.501(6) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.406(6) . ?
C6 C11 1.411(6) . ?
C6 N1 1.448(5) . ?
C7 C8 1.406(6) . ?
C7 C12 1.522(7) . ?
C8 C9 1.372(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.381(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.392(6) . ?
C10 H10 0.9500 . ?
C11 C15 1.518(6) . ?
C12 C13 1.523(6) . ?
C12 C14 1.527(6) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.524(6) . ?
C15 C16 1.535(6) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C23 1.401(6) . ?
C18 C19 1.411(6) . ?
C18 N2 1.463(5) . ?
C19 C20 1.391(6) . ?
C19 C24 1.517(6) . ?
C20 C21 1.372(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.383(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.378(6) . ?
C22 H22 0.9500 . ?
C23 C27 1.524(6) . ?
C24 C25 1.527(6) . ?
C24 C26 1.530(7) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.523(6) . ?
C27 C29 1.530(6) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N3 1.397(5) . ?
C30 C35 1.413(6) . ?
C30 C31 1.428(6) . ?
C31 C32 1.382(6) . ?
C31 C36 1.512(6) . ?
C32 C33 1.387(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.379(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.386(6) . ?
C34 H34 0.9500 . ?
C35 C39 1.527(6) . ?
C36 C37 1.527(6) . ?
C36 C38 1.531(6) . ?
C36 H36 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C41 1.537(7) . ?
C39 C40 1.542(6) . ?
C39 H39 1.0000 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 N4 1.484(5) . ?
C42 C43 1.515(6) . ?
C42 C45 1.531(6) . ?
C42 C44 1.540(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 O2 1.205(5) . ?
C46 O1 1.345(5) . ?
C46 N4 1.391(5) . ?
C46 Nb 2.575(4) . ?
C47 C48 1.423(13) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 O3 1.458(10) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 O3 1.322(9) . ?
C49 C50 1.444(11) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
N1 Nb 2.097(3) . ?
N2 Nb 2.211(3) . ?
N3 Nb 1.789(3) . ?
N4 Nb 2.071(3) . ?
O1 Nb 2.070(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.7(4) . . ?
N1 C1 C4 119.6(3) . . ?
C2 C1 C4 117.6(4) . . ?
C1 C2 C3 129.0(4) . . ?
C1 C2 H2 115.5 . . ?
C3 C2 H2 115.5 . . ?
N2 C3 C2 124.0(4) . . ?
N2 C3 C5 120.4(4) . . ?
C2 C3 C5 115.6(4) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 121.9(4) . . ?
C7 C6 N1 120.1(3) . . ?
C11 C6 N1 118.0(3) . . ?
C6 C7 C8 117.7(4) . . ?
C6 C7 C12 123.5(4) . . ?
C8 C7 C12 118.9(4) . . ?
C9 C8 C7 120.9(4) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C8 C9 C10 120.6(4) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C9 C10 C11 121.4(4) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C10 C11 C6 117.5(4) . . ?
C10 C11 C15 121.1(4) . . ?
C6 C11 C15 121.4(4) . . ?
C7 C12 C13 112.4(4) . . ?
C7 C12 C14 111.1(4) . . ?
C13 C12 C14 109.5(4) . . ?
C7 C12 H12 107.9 . . ?
C13 C12 H12 107.9 . . ?
C14 C12 H12 107.9 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C17 113.3(4) . . ?
C11 C15 C16 110.7(4) . . ?
C17 C15 C16 110.3(3) . . ?
C11 C15 H15 107.4 . . ?
C17 C15 H15 107.4 . . ?
C16 C15 H15 107.4 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 121.7(4) . . ?
C23 C18 N2 120.2(4) . . ?
C19 C18 N2 118.0(4) . . ?
C20 C19 C18 117.2(4) . . ?
C20 C19 C24 120.2(4) . . ?
C18 C19 C24 122.6(4) . . ?
C21 C20 C19 121.5(4) . . ?
C21 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
C20 C21 C22 120.3(4) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C23 C22 C21 120.9(4) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C18 118.3(4) . . ?
C22 C23 C27 119.3(4) . . ?
C18 C23 C27 122.4(4) . . ?
C19 C24 C25 111.7(4) . . ?
C19 C24 C26 110.7(4) . . ?
C25 C24 C26 110.4(4) . . ?
C19 C24 H24 108.0 . . ?
C25 C24 H24 108.0 . . ?
C26 C24 H24 108.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C23 110.8(3) . . ?
C28 C27 C29 110.4(4) . . ?
C23 C27 C29 112.3(4) . . ?
C28 C27 H27 107.7 . . ?
C23 C27 H27 107.7 . . ?
C29 C27 H27 107.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C35 120.7(4) . . ?
N3 C30 C31 119.9(3) . . ?
C35 C30 C31 119.4(4) . . ?
C32 C31 C30 118.4(4) . . ?
C32 C31 C36 119.3(4) . . ?
C30 C31 C36 122.3(4) . . ?
C31 C32 C33 122.3(4) . . ?
C31 C32 H32 118.9 . . ?
C33 C32 H32 118.9 . . ?
C34 C33 C32 118.9(4) . . ?
C34 C33 H33 120.6 . . ?
C32 C33 H33 120.6 . . ?
C33 C34 C35 121.8(4) . . ?
C33 C34 H34 119.1 . . ?
C35 C34 H34 119.1 . . ?
C34 C35 C30 119.2(4) . . ?
C34 C35 C39 119.1(4) . . ?
C30 C35 C39 121.7(4) . . ?
C31 C36 C37 112.0(4) . . ?
C31 C36 C38 110.7(4) . . ?
C37 C36 C38 109.0(4) . . ?
C31 C36 H36 108.4 . . ?
C37 C36 H36 108.4 . . ?
C38 C36 H36 108.4 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C39 C41 113.1(4) . . ?
C35 C39 C40 110.3(3) . . ?
C41 C39 C40 108.9(4) . . ?
C35 C39 H39 108.1 . . ?
C41 C39 H39 108.1 . . ?
C40 C39 H39 108.1 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N4 C42 C43 107.9(3) . . ?
N4 C42 C45 109.8(3) . . ?
C43 C42 C45 109.4(4) . . ?
N4 C42 C44 110.4(3) . . ?
C43 C42 C44 109.9(4) . . ?
C45 C42 C44 109.6(3) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O2 C46 O1 124.2(4) . . ?
O2 C46 N4 129.4(4) . . ?
O1 C46 N4 106.4(3) . . ?
O2 C46 Nb 175.9(3) . . ?
O1 C46 Nb 53.13(19) . . ?
N4 C46 Nb 53.4(2) . . ?
C48 C47 H47A 109.5 . . ?
C48 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C48 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C47 C48 O3 112.0(6) . . ?
C47 C48 H48A 109.2 . . ?
O3 C48 H48A 109.2 . . ?
C47 C48 H48B 109.2 . . ?
O3 C48 H48B 109.2 . . ?
H48A C48 H48B 107.9 . . ?
O3 C49 C50 115.7(6) . . ?
O3 C49 H49A 108.4 . . ?
C50 C49 H49A 108.4 . . ?
O3 C49 H49B 108.4 . . ?
C50 C49 H49B 108.4 . . ?
H49A C49 H49B 107.4 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C1 N1 C6 120.7(3) . . ?
C1 N1 Nb 128.2(3) . . ?
C6 N1 Nb 111.0(2) . . ?
C3 N2 C18 116.2(3) . . ?
C3 N2 Nb 124.1(3) . . ?
C18 N2 Nb 119.7(2) . . ?
C30 N3 Nb 174.2(3) . . ?
C46 N4 C42 118.9(3) . . ?
C46 N4 Nb 94.0(3) . . ?
C42 N4 Nb 146.2(3) . . ?
C46 O1 Nb 95.5(2) . . ?
C49 O3 C48 121.2(7) . . ?
N3 Nb O1 125.64(13) . . ?
N3 Nb N4 108.89(14) . . ?
O1 Nb N4 63.89(11) . . ?
N3 Nb N1 104.93(13) . . ?
O1 Nb N1 127.99(12) . . ?
N4 Nb N1 113.56(12) . . ?
N3 Nb N2 99.33(14) . . ?
O1 Nb N2 76.71(11) . . ?
N4 Nb N2 139.96(13) . . ?
N1 Nb N2 84.65(12) . . ?
N3 Nb C46 123.78(14) . . ?
O1 Nb C46 31.34(12) . . ?
N4 Nb C46 32.61(13) . . ?
N1 Nb C46 125.57(13) . . ?
N2 Nb C46 107.59(13) . . ?

_refine_diff_density_max         0.623
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.053


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Diethyl ether'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2004310'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-17 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
hydrido-(tert-butyl)amino-(tert-butyl)imino-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V)
_chemical_name_common            (BDI)NbH(NHtBu)(NtBu)
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H61 N4 Nb'
_chemical_formula_sum            'C37 H61 N4 Nb'
_chemical_formula_weight         654.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.322(5)
_cell_length_b                   12.754(5)
_cell_length_c                   21.266(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 91.766(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     3612(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9783
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      25.47

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_F_000             1408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.362
_shelx_estimated_absorpt_T_min   0.931
_shelx_estimated_absorpt_T_max   0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6810
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            70529
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.529
_diffrn_reflns_theta_max         25.469
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6652
_reflns_number_gt                6122
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXT
_computing_structure_refinement  SHELXL-2014
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+30.5505P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6652
_refine_ls_number_parameters     436
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0660
_refine_ls_wR_factor_ref         0.1500
_refine_ls_wR_factor_gt          0.1485
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7660(4) 0.3476(4) 0.5321(2) 0.0206(10) Uani 1 1 d . . . . .
C2 C 0.6849(4) 0.2902(4) 0.5085(2) 0.0222(10) Uani 1 1 d . . . . .
H2 H 0.6647 0.3049 0.4662 0.027 Uiso 1 1 calc R U . . .
C3 C 0.6291(4) 0.2138(4) 0.5387(2) 0.0194(10) Uani 1 1 d . . . . .
C4 C 0.8238(4) 0.4112(4) 0.4859(2) 0.0269(11) Uani 1 1 d . . . . .
H4A H 0.8066 0.4855 0.4903 0.040 Uiso 1 1 calc R U . . .
H4B H 0.8066 0.3879 0.4430 0.040 Uiso 1 1 calc R U . . .
H4C H 0.8960 0.4018 0.4943 0.040 Uiso 1 1 calc R U . . .
C5 C 0.5716(4) 0.1391(4) 0.4953(2) 0.0285(12) Uani 1 1 d . . . . .
H5A H 0.5470 0.0797 0.5197 0.043 Uiso 1 1 calc R U . . .
H5B H 0.6161 0.1133 0.4628 0.043 Uiso 1 1 calc R U . . .
H5C H 0.5145 0.1759 0.4753 0.043 Uiso 1 1 calc R U . . .
C6 C 0.8958(3) 0.3801(4) 0.6092(2) 0.0203(10) Uani 1 1 d . . . . .
C7 C 0.9195(4) 0.4830(4) 0.6276(2) 0.0253(11) Uani 1 1 d . . . . .
C8 C 1.0197(4) 0.5085(5) 0.6422(2) 0.0311(12) Uani 1 1 d . . . . .
H8 H 1.0364 0.5780 0.6548 0.037 Uiso 1 1 calc R U . . .
C9 C 1.0939(4) 0.4348(5) 0.6388(3) 0.0335(13) Uani 1 1 d . . . . .
H9 H 1.1614 0.4532 0.6493 0.040 Uiso 1 1 calc R U . . .
C10 C 1.0709(4) 0.3338(5) 0.6202(2) 0.0315(12) Uani 1 1 d . . . . .
H10 H 1.1233 0.2835 0.6176 0.038 Uiso 1 1 calc R U . . .
C11 C 0.9725(4) 0.3040(4) 0.6050(2) 0.0252(11) Uani 1 1 d . . . . .
C12 C 0.8428(4) 0.5700(4) 0.6314(2) 0.0289(12) Uani 1 1 d . . . . .
H12 H 0.7751 0.5394 0.6215 0.035 Uiso 1 1 calc R U . . .
C13 C 0.8620(5) 0.6564(5) 0.5831(3) 0.0394(14) Uani 1 1 d . . . . .
H13A H 0.9271 0.6895 0.5928 0.059 Uiso 1 1 calc R U . . .
H13B H 0.8087 0.7092 0.5848 0.059 Uiso 1 1 calc R U . . .
H13C H 0.8626 0.6257 0.5409 0.059 Uiso 1 1 calc R U . . .
C14 C 0.8408(5) 0.6186(4) 0.6976(3) 0.0391(14) Uani 1 1 d . . . . .
H14A H 0.8304 0.5631 0.7287 0.059 Uiso 1 1 calc R U . . .
H14B H 0.7860 0.6696 0.6993 0.059 Uiso 1 1 calc R U . . .
H14C H 0.9049 0.6538 0.7071 0.059 Uiso 1 1 calc R U . . .
C15 C 0.9512(4) 0.1920(4) 0.5836(2) 0.0286(11) Uani 1 1 d . . . . .
H15 H 0.8776 0.1790 0.5877 0.034 Uiso 1 1 calc R U . . .
C16 C 0.9763(5) 0.1747(5) 0.5147(3) 0.0453(16) Uani 1 1 d . . . . .
H16A H 0.9332 0.2195 0.4878 0.068 Uiso 1 1 calc R U . . .
H16B H 0.9649 0.1011 0.5035 0.068 Uiso 1 1 calc R U . . .
H16C H 1.0468 0.1927 0.5085 0.068 Uiso 1 1 calc R U . . .
C17 C 1.0072(5) 0.1107(5) 0.6239(3) 0.0481(16) Uani 1 1 d . . . . .
H17A H 1.0797 0.1187 0.6186 0.072 Uiso 1 1 calc R U . . .
H17B H 0.9864 0.0402 0.6107 0.072 Uiso 1 1 calc R U . . .
H17C H 0.9917 0.1211 0.6682 0.072 Uiso 1 1 calc R U . . .
C18 C 0.5718(4) 0.1146(4) 0.6252(2) 0.0214(10) Uani 1 1 d . . . . .
C19 C 0.6268(4) 0.0228(4) 0.6409(2) 0.0262(11) Uani 1 1 d . . . . .
C20 C 0.5740(5) -0.0640(4) 0.6627(2) 0.0321(13) Uani 1 1 d . . . . .
H20 H 0.6094 -0.1266 0.6730 0.038 Uiso 1 1 calc R U . . .
C21 C 0.4714(4) -0.0606(4) 0.6696(2) 0.0333(13) Uani 1 1 d . . . . .
H21 H 0.4366 -0.1204 0.6842 0.040 Uiso 1 1 calc R U . . .
C22 C 0.4197(4) 0.0303(4) 0.6552(2) 0.0318(12) Uani 1 1 d . . . . .
H22 H 0.3491 0.0322 0.6603 0.038 Uiso 1 1 calc R U . . .
C23 C 0.4675(4) 0.1192(4) 0.6333(2) 0.0272(11) Uani 1 1 d . . . . .
C24 C 0.7393(4) 0.0157(4) 0.6337(3) 0.0307(12) Uani 1 1 d . . . . .
H24 H 0.7671 0.0884 0.6364 0.037 Uiso 1 1 calc R U . . .
C25 C 0.7897(5) -0.0491(5) 0.6869(3) 0.0437(15) Uani 1 1 d . . . . .
H25A H 0.7660 -0.0248 0.7275 0.066 Uiso 1 1 calc R U . . .
H25B H 0.8627 -0.0405 0.6857 0.066 Uiso 1 1 calc R U . . .
H25C H 0.7725 -0.1233 0.6812 0.066 Uiso 1 1 calc R U . . .
C26 C 0.7666(5) -0.0299(5) 0.5699(3) 0.0430(15) Uani 1 1 d . . . . .
H26A H 0.7324 -0.0973 0.5636 0.064 Uiso 1 1 calc R U . . .
H26B H 0.8394 -0.0404 0.5690 0.064 Uiso 1 1 calc R U . . .
H26C H 0.7455 0.0188 0.5364 0.064 Uiso 1 1 calc R U . . .
C27 C 0.4073(4) 0.2176(5) 0.6207(3) 0.0304(12) Uani 1 1 d . . . . .
H27 H 0.4549 0.2751 0.6100 0.036 Uiso 1 1 calc R U . . .
C28 C 0.3311(5) 0.2045(7) 0.5652(3) 0.0532(19) Uani 1 1 d . . . . .
H28A H 0.3667 0.1852 0.5272 0.080 Uiso 1 1 calc R U . . .
H28B H 0.2952 0.2707 0.5579 0.080 Uiso 1 1 calc R U . . .
H28C H 0.2829 0.1493 0.5751 0.080 Uiso 1 1 calc R U . . .
C29 C 0.3512(5) 0.2505(5) 0.6790(3) 0.0386(14) Uani 1 1 d . . . . .
H29A H 0.3042 0.1950 0.6904 0.058 Uiso 1 1 calc R U . . .
H29B H 0.3139 0.3154 0.6702 0.058 Uiso 1 1 calc R U . . .
H29C H 0.3994 0.2624 0.7140 0.058 Uiso 1 1 calc R U . . .
C30 C 0.5351(4) 0.5330(4) 0.6326(3) 0.0325(13) Uani 1 1 d . . . . .
C34 C 0.8196(4) 0.3079(4) 0.7836(2) 0.0250(11) Uani 1 1 d . . . . .
N1 N 0.7934(3) 0.3493(3) 0.59370(17) 0.0175(8) Uani 1 1 d . . . . .
N2 N 0.6255(3) 0.2044(3) 0.60061(18) 0.0201(8) Uani 1 1 d . . . . .
Nb Nb 0.67740(3) 0.33606(3) 0.66542(2) 0.01515(13) Uani 1 1 d . . . . .
C31 C 0.4294(7) 0.5009(8) 0.6197(5) 0.048(2) Uani 0.660(4) 1 d . . P A 1
H31A H 0.4016 0.4714 0.6580 0.071 Uiso 0.660(4) 1 calc R U P A 1
H31B H 0.4270 0.4480 0.5863 0.071 Uiso 0.660(4) 1 calc R U P A 1
H31C H 0.3897 0.5622 0.6064 0.071 Uiso 0.660(4) 1 calc R U P A 1
C32 C 0.5769(7) 0.5747(9) 0.5684(5) 0.051(3) Uani 0.660(4) 1 d . . P A 1
H32A H 0.5265 0.6199 0.5476 0.077 Uiso 0.660(4) 1 calc R U P A 1
H32B H 0.5914 0.5151 0.5411 0.077 Uiso 0.660(4) 1 calc R U P A 1
H32C H 0.6386 0.6148 0.5769 0.077 Uiso 0.660(4) 1 calc R U P A 1
C33 C 0.5487(10) 0.6164(9) 0.6796(6) 0.064(4) Uani 0.660(4) 1 d . . P A 1
H33A H 0.5084 0.6006 0.7162 0.096 Uiso 0.660(4) 1 calc R U P A 1
H33B H 0.5270 0.6835 0.6613 0.096 Uiso 0.660(4) 1 calc R U P A 1
H33C H 0.6197 0.6208 0.6927 0.096 Uiso 0.660(4) 1 calc R U P A 1
N3 N 0.5979(4) 0.4411(5) 0.6486(3) 0.0172(9) Uani 0.660(4) 1 d . . P A 1
C35 C 0.9221(14) 0.3589(12) 0.7880(9) 0.031(3) Uani 0.660(4) 1 d . . P A 1
H35A H 0.9162 0.4291 0.8062 0.046 Uiso 0.660(4) 1 calc R U P A 1
H35B H 0.9493 0.3645 0.7458 0.046 Uiso 0.660(4) 1 calc R U P A 1
H35C H 0.9673 0.3162 0.8147 0.046 Uiso 0.660(4) 1 calc R U P A 1
C36 C 0.7731(6) 0.2889(7) 0.8442(4) 0.0304(16) Uani 0.660(4) 1 d . . P A 1
H36A H 0.8181 0.2459 0.8709 0.046 Uiso 0.660(4) 1 calc R U P A 1
H36B H 0.7092 0.2521 0.8372 0.046 Uiso 0.660(4) 1 calc R U P A 1
H36C H 0.7610 0.3560 0.8651 0.046 Uiso 0.660(4) 1 calc R U P A 1
C37 C 0.8275(7) 0.2042(6) 0.7445(4) 0.0323(17) Uani 0.660(4) 1 d . . P A 1
H37A H 0.8779 0.1581 0.7645 0.048 Uiso 0.660(4) 1 calc R U P A 1
H37B H 0.8473 0.2210 0.7017 0.048 Uiso 0.660(4) 1 calc R U P A 1
H37C H 0.7621 0.1688 0.7430 0.048 Uiso 0.660(4) 1 calc R U P A 1
N4 N 0.7529(6) 0.3769(5) 0.7418(3) 0.0172(9) Uani 0.660(4) 1 d . . P A 1
H4 H 0.7475 0.4429 0.7534 0.021 Uiso 0.660(4) 1 calc R U P A 1
C31A C 0.4283(14) 0.5305(16) 0.6725(11) 0.048(2) Uani 0.340(4) 1 d . . P A 2
H31D H 0.3744 0.5640 0.6474 0.071 Uiso 0.340(4) 1 calc R U P A 2
H31E H 0.4383 0.5683 0.7123 0.071 Uiso 0.340(4) 1 calc R U P A 2
H31F H 0.4100 0.4576 0.6811 0.071 Uiso 0.340(4) 1 calc R U P A 2
C32A C 0.5269(15) 0.4946(15) 0.5748(8) 0.044(5) Uani 0.340(4) 1 d . . P A 2
H32D H 0.5878 0.5108 0.5521 0.066 Uiso 0.340(4) 1 calc R U P A 2
H32E H 0.4686 0.5261 0.5528 0.066 Uiso 0.340(4) 1 calc R U P A 2
H32F H 0.5180 0.4184 0.5768 0.066 Uiso 0.340(4) 1 calc R U P A 2
C33A C 0.569(2) 0.6508(18) 0.6397(12) 0.064(4) Uani 0.340(4) 1 d . . P A 2
H33D H 0.6277 0.6634 0.6144 0.096 Uiso 0.340(4) 1 calc R U P A 2
H33E H 0.5853 0.6657 0.6840 0.096 Uiso 0.340(4) 1 calc R U P A 2
H33F H 0.5137 0.6967 0.6251 0.096 Uiso 0.340(4) 1 calc R U P A 2
N3A N 0.6064(9) 0.4729(9) 0.6792(6) 0.0172(9) Uani 0.340(4) 1 d . . P A 2
H3A H 0.6170 0.5024 0.7162 0.021 Uiso 0.340(4) 1 calc R U P A 2
C35A C 0.933(3) 0.324(3) 0.7773(19) 0.043(9) Uani 0.340(4) 1 d . . P A 2
H35D H 0.9578 0.2744 0.7462 0.064 Uiso 0.340(4) 1 calc R U P A 2
H35E H 0.9668 0.3117 0.8181 0.064 Uiso 0.340(4) 1 calc R U P A 2
H35F H 0.9454 0.3958 0.7634 0.064 Uiso 0.340(4) 1 calc R U P A 2
C36A C 0.7960(12) 0.3770(14) 0.8462(7) 0.0304(16) Uani 0.340(4) 1 d . . P A 2
H36D H 0.8070 0.4515 0.8374 0.046 Uiso 0.340(4) 1 calc R U P A 2
H36E H 0.8409 0.3549 0.8811 0.046 Uiso 0.340(4) 1 calc R U P A 2
H36F H 0.7261 0.3660 0.8576 0.046 Uiso 0.340(4) 1 calc R U P A 2
C37A C 0.7974(13) 0.1948(12) 0.8043(7) 0.0323(17) Uani 0.340(4) 1 d . . P A 2
H37D H 0.7248 0.1858 0.8081 0.048 Uiso 0.340(4) 1 calc R U P A 2
H37E H 0.8311 0.1812 0.8451 0.048 Uiso 0.340(4) 1 calc R U P A 2
H37F H 0.8222 0.1456 0.7730 0.048 Uiso 0.340(4) 1 calc R U P A 2
N4A N 0.7602(12) 0.3403(10) 0.7356(7) 0.0172(9) Uani 0.340(4) 1 d . . P A 2
H1 H 0.597(4) 0.255(5) 0.709(3) 0.035(16) Uiso 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.349(6) . ?
C1 C2 1.386(7) . ?
C1 C4 1.505(6) . ?
C2 C3 1.394(7) . ?
C2 H2 0.9500 . ?
C3 N2 1.325(6) . ?
C3 C5 1.517(6) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.403(7) . ?
C6 C11 1.414(7) . ?
C6 N1 1.447(6) . ?
C7 C8 1.399(7) . ?
C7 C12 1.512(8) . ?
C8 C9 1.368(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.380(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.394(7) . ?
C10 H10 0.9500 . ?
C11 C15 1.524(7) . ?
C12 C13 1.533(7) . ?
C12 C14 1.539(7) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.524(8) . ?
C15 C16 1.530(7) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C23 1.407(7) . ?
C18 C19 1.415(7) . ?
C18 N2 1.456(6) . ?
C19 C20 1.399(7) . ?
C19 C24 1.513(8) . ?
C20 C21 1.380(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.379(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.387(7) . ?
C22 H22 0.9500 . ?
C23 C27 1.509(8) . ?
C24 C26 1.530(8) . ?
C24 C25 1.537(7) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C29 1.528(8) . ?
C27 C28 1.542(8) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C32A 1.324(18) . ?
C30 C33 1.467(12) . ?
C30 N3 1.475(7) . ?
C30 C31 1.484(11) . ?
C30 N3A 1.554(12) . ?
C30 C33A 1.57(2) . ?
C30 C32 1.581(11) . ?
C30 C31A 1.68(2) . ?
C34 N4A 1.339(16) . ?
C34 C36 1.467(9) . ?
C34 N4 1.519(8) . ?
C34 C35 1.51(2) . ?
C34 C35A 1.53(4) . ?
C34 C37A 1.539(17) . ?
C34 C37 1.566(9) . ?
C34 C36A 1.635(16) . ?
N1 Nb 2.211(4) . ?
N2 Nb 2.266(4) . ?
Nb N3 1.738(6) . ?
Nb N4A 1.829(15) . ?
Nb N4 1.955(7) . ?
Nb N3A 2.011(12) . ?
Nb H1 1.76(6) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
N4 H4 0.8800 . ?
C31A H31D 0.9800 . ?
C31A H31E 0.9800 . ?
C31A H31F 0.9800 . ?
C32A H32D 0.9800 . ?
C32A H32E 0.9800 . ?
C32A H32F 0.9800 . ?
C33A H33D 0.9800 . ?
C33A H33E 0.9800 . ?
C33A H33F 0.9800 . ?
N3A H3A 0.8800 . ?
C35A H35D 0.9800 . ?
C35A H35E 0.9800 . ?
C35A H35F 0.9800 . ?
C36A H36D 0.9800 . ?
C36A H36E 0.9800 . ?
C36A H36F 0.9800 . ?
C37A H37D 0.9800 . ?
C37A H37E 0.9800 . ?
C37A H37F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.0(4) . . ?
N1 C1 C4 119.7(4) . . ?
C2 C1 C4 117.2(4) . . ?
C1 C2 C3 128.5(4) . . ?
C1 C2 H2 115.7 . . ?
C3 C2 H2 115.7 . . ?
N2 C3 C2 123.8(4) . . ?
N2 C3 C5 121.0(4) . . ?
C2 C3 C5 115.2(4) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 120.2(5) . . ?
C7 C6 N1 121.3(4) . . ?
C11 C6 N1 118.5(4) . . ?
C8 C7 C6 118.9(5) . . ?
C8 C7 C12 117.4(5) . . ?
C6 C7 C12 123.7(5) . . ?
C9 C8 C7 121.0(5) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C10 120.2(5) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C11 121.3(5) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C6 118.4(5) . . ?
C10 C11 C15 119.3(5) . . ?
C6 C11 C15 122.3(5) . . ?
C7 C12 C13 111.4(5) . . ?
C7 C12 C14 112.0(5) . . ?
C13 C12 C14 109.4(4) . . ?
C7 C12 H12 108.0 . . ?
C13 C12 H12 108.0 . . ?
C14 C12 H12 108.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C17 112.7(5) . . ?
C11 C15 C16 112.1(5) . . ?
C17 C15 C16 108.8(5) . . ?
C11 C15 H15 107.7 . . ?
C17 C15 H15 107.7 . . ?
C16 C15 H15 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 120.8(4) . . ?
C23 C18 N2 120.6(4) . . ?
C19 C18 N2 118.6(4) . . ?
C20 C19 C18 118.0(5) . . ?
C20 C19 C24 119.7(5) . . ?
C18 C19 C24 122.3(4) . . ?
C21 C20 C19 121.4(5) . . ?
C21 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
C22 C21 C20 119.5(5) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C21 C22 C23 122.1(5) . . ?
C21 C22 H22 119.0 . . ?
C23 C22 H22 119.0 . . ?
C22 C23 C18 118.2(5) . . ?
C22 C23 C27 119.5(5) . . ?
C18 C23 C27 122.3(5) . . ?
C19 C24 C26 112.0(5) . . ?
C19 C24 C25 111.7(5) . . ?
C26 C24 C25 109.7(5) . . ?
C19 C24 H24 107.7 . . ?
C26 C24 H24 107.7 . . ?
C25 C24 H24 107.7 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 C29 110.7(5) . . ?
C23 C27 C28 112.3(5) . . ?
C29 C27 C28 108.9(5) . . ?
C23 C27 H27 108.2 . . ?
C29 C27 H27 108.2 . . ?
C28 C27 H27 108.2 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C33 C30 N3 111.2(6) . . ?
C33 C30 C31 115.0(8) . . ?
N3 C30 C31 110.6(6) . . ?
C32A C30 N3A 116.1(10) . . ?
C32A C30 C33A 117.3(13) . . ?
N3A C30 C33A 104.1(10) . . ?
C33 C30 C32 107.8(8) . . ?
N3 C30 C32 104.8(6) . . ?
C31 C30 C32 106.9(7) . . ?
C32A C30 C31A 114.5(12) . . ?
N3A C30 C31A 100.3(9) . . ?
C33A C30 C31A 102.3(13) . . ?
C36 C34 N4 110.7(5) . . ?
C36 C34 C35 115.0(9) . . ?
N4 C34 C35 107.3(8) . . ?
N4A C34 C35A 116.8(18) . . ?
N4A C34 C37A 113.2(9) . . ?
C35A C34 C37A 110.4(15) . . ?
C36 C34 C37 111.3(6) . . ?
N4 C34 C37 103.1(5) . . ?
C35 C34 C37 108.7(7) . . ?
N4A C34 C36A 109.3(8) . . ?
C35A C34 C36A 102.4(15) . . ?
C37A C34 C36A 103.2(9) . . ?
C1 N1 C6 116.8(4) . . ?
C1 N1 Nb 119.6(3) . . ?
C6 N1 Nb 122.5(3) . . ?
C3 N2 C18 117.4(4) . . ?
C3 N2 Nb 121.2(3) . . ?
C18 N2 Nb 120.6(3) . . ?
N3 Nb N4 105.1(3) . . ?
N4A Nb N3A 97.5(5) . . ?
N3 Nb N1 103.5(2) . . ?
N4A Nb N1 98.2(5) . . ?
N4 Nb N1 101.6(2) . . ?
N3A Nb N1 112.1(3) . . ?
N3 Nb N2 105.9(2) . . ?
N4A Nb N2 133.1(4) . . ?
N4 Nb N2 147.4(2) . . ?
N3A Nb N2 126.5(4) . . ?
N1 Nb N2 81.02(14) . . ?
N3 Nb H1 100.6(19) . . ?
N4A Nb H1 87.1(19) . . ?
N4 Nb H1 91.4(18) . . ?
N3A Nb H1 97.8(19) . . ?
N1 Nb H1 148.4(19) . . ?
N2 Nb H1 73.0(19) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 N3 Nb 176.8(5) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 N4 Nb 127.5(4) . . ?
C34 N4 H4 116.3 . . ?
Nb N4 H4 116.3 . . ?
C30 C31A H31D 109.5 . . ?
C30 C31A H31E 109.5 . . ?
H31D C31A H31E 109.5 . . ?
C30 C31A H31F 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
C30 C32A H32D 109.5 . . ?
C30 C32A H32E 109.5 . . ?
H32D C32A H32E 109.5 . . ?
C30 C32A H32F 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?
C30 C33A H33D 109.5 . . ?
C30 C33A H33E 109.5 . . ?
H33D C33A H33E 109.5 . . ?
C30 C33A H33F 109.5 . . ?
H33D C33A H33F 109.5 . . ?
H33E C33A H33F 109.5 . . ?
C30 N3A Nb 128.1(8) . . ?
C30 N3A H3A 116.0 . . ?
Nb N3A H3A 116.0 . . ?
C34 C35A H35D 109.5 . . ?
C34 C35A H35E 109.5 . . ?
H35D C35A H35E 109.5 . . ?
C34 C35A H35F 109.5 . . ?
H35D C35A H35F 109.5 . . ?
H35E C35A H35F 109.5 . . ?
C34 C36A H36D 109.5 . . ?
C34 C36A H36E 109.5 . . ?
H36D C36A H36E 109.5 . . ?
C34 C36A H36F 109.5 . . ?
H36D C36A H36F 109.5 . . ?
H36E C36A H36F 109.5 . . ?
C34 C37A H37D 109.5 . . ?
C34 C37A H37E 109.5 . . ?
H37D C37A H37E 109.5 . . ?
C34 C37A H37F 109.5 . . ?
H37D C37A H37F 109.5 . . ?
H37E C37A H37F 109.5 . . ?
C34 N4A Nb 160.2(10) . . ?

_refine_diff_density_max         1.210
_refine_diff_density_min         -1.496
_refine_diff_density_rms         0.121


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexamethyldisiloxane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2004313'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-17 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
Formato-(N-(tert-butyl)-1-phenylsilyl)amino-(tert-butyl)imino-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V)
_chemical_name_common            (BDI)Nb(OC(H)O)(N[SiH2nBu]tBu)(NtBu)
_chemical_melting_point          396
_chemical_formula_moiety         'C42 H71 N4 Nb O2 Si'
_chemical_formula_sum            'C42 H71 N4 Nb O2 Si'
_chemical_formula_weight         785.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.6503(7)
_cell_length_b                   24.6381(15)
_cell_length_c                   16.5787(11)
_cell_angle_alpha                90
_cell_angle_beta                 97.111(3)
_cell_angle_gamma                90
_cell_volume                     4316.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9935
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      25.35

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_F_000             1688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.344
_shelx_estimated_absorpt_T_min   0.973
_shelx_estimated_absorpt_T_max   0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7031
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   TWINABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            9146
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.488
_diffrn_reflns_theta_max         25.428
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9146
_reflns_number_gt                8330
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR-92
_computing_structure_refinement  SHELXL-2014
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_refine_special_details          'Refined as a 2-component twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0535P)²+3.0907P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9146
_refine_ls_number_parameters     477
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0995
_refine_ls_wR_factor_gt          0.0948
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0044(2) 0.35747(10) 0.32694(15) 0.0139(5) Uani 1 1 d . . . . .
C2 C 1.0457(2) 0.39356(10) 0.27224(16) 0.0144(5) Uani 1 1 d . . . . .
H2 H 1.1248 0.4103 0.2895 0.017 Uiso 1 1 calc R U . . .
C3 C 0.9878(2) 0.40930(10) 0.19426(16) 0.0155(5) Uani 1 1 d . . . . .
C4 C 1.1030(2) 0.34085(11) 0.39625(17) 0.0202(6) Uani 1 1 d . . . . .
H4A H 1.1014 0.3663 0.4416 0.030 Uiso 1 1 calc R U . . .
H4B H 1.1869 0.3414 0.3778 0.030 Uiso 1 1 calc R U . . .
H4C H 1.0845 0.3041 0.4142 0.030 Uiso 1 1 calc R U . . .
C5 C 1.0766(2) 0.43414(11) 0.13984(16) 0.0204(6) Uani 1 1 d . . . . .
H5A H 1.0407 0.4299 0.0829 0.031 Uiso 1 1 calc R U . . .
H5B H 1.1588 0.4158 0.1489 0.031 Uiso 1 1 calc R U . . .
H5C H 1.0877 0.4728 0.1525 0.031 Uiso 1 1 calc R U . . .
C6 C 0.8749(2) 0.28482(10) 0.36213(16) 0.0159(5) Uani 1 1 d . . . . .
C7 C 0.8414(3) 0.28103(10) 0.44147(16) 0.0187(6) Uani 1 1 d . . . . .
C8 C 0.8414(3) 0.23010(11) 0.47820(18) 0.0240(6) Uani 1 1 d . . . . .
H8 H 0.8193 0.2273 0.5318 0.029 Uiso 1 1 calc R U . . .
C9 C 0.8726(3) 0.18363(11) 0.43872(19) 0.0275(7) Uani 1 1 d . . . . .
H9 H 0.8718 0.1493 0.4647 0.033 Uiso 1 1 calc R U . . .
C10 C 0.9050(3) 0.18786(11) 0.36082(18) 0.0242(6) Uani 1 1 d . . . . .
H10 H 0.9267 0.1559 0.3335 0.029 Uiso 1 1 calc R U . . .
C11 C 0.9067(3) 0.23763(10) 0.32125(17) 0.0201(6) Uani 1 1 d . . . . .
C12 C 0.8085(3) 0.32977(11) 0.49144(16) 0.0192(6) Uani 1 1 d . . . . .
H12 H 0.8004 0.3625 0.4554 0.023 Uiso 1 1 calc R U . . .
C13 C 0.9111(3) 0.34078(12) 0.56275(18) 0.0260(6) Uani 1 1 d . . . . .
H13A H 0.9186 0.3094 0.5993 0.039 Uiso 1 1 calc R U . . .
H13B H 0.8882 0.3729 0.5925 0.039 Uiso 1 1 calc R U . . .
H13C H 0.9922 0.3471 0.5421 0.039 Uiso 1 1 calc R U . . .
C14 C 0.6834(3) 0.32132(12) 0.52602(18) 0.0266(6) Uani 1 1 d . . . . .
H14A H 0.6168 0.3124 0.4818 0.040 Uiso 1 1 calc R U . . .
H14B H 0.6606 0.3547 0.5530 0.040 Uiso 1 1 calc R U . . .
H14C H 0.6925 0.2915 0.5655 0.040 Uiso 1 1 calc R U . . .
C15 C 0.9505(3) 0.23900(11) 0.23718(17) 0.0214(6) Uani 1 1 d . . . . .
H15 H 0.9261 0.2749 0.2119 0.026 Uiso 1 1 calc R U . . .
C16 C 1.0952(3) 0.23401(13) 0.2444(2) 0.0311(7) Uani 1 1 d . . . . .
H16A H 1.1340 0.2633 0.2788 0.047 Uiso 1 1 calc R U . . .
H16B H 1.1226 0.2366 0.1903 0.047 Uiso 1 1 calc R U . . .
H16C H 1.1213 0.1989 0.2688 0.047 Uiso 1 1 calc R U . . .
C17 C 0.8890(3) 0.19430(12) 0.18096(19) 0.0300(7) Uani 1 1 d . . . . .
H17A H 0.9170 0.1587 0.2025 0.045 Uiso 1 1 calc R U . . .
H17B H 0.9140 0.1989 0.1264 0.045 Uiso 1 1 calc R U . . .
H17C H 0.7967 0.1968 0.1781 0.045 Uiso 1 1 calc R U . . .
C18 C 0.8192(2) 0.41862(11) 0.08649(16) 0.0168(5) Uani 1 1 d . . . . .
C19 C 0.7936(3) 0.37813(11) 0.02805(16) 0.0197(6) Uani 1 1 d . . . . .
C20 C 0.7418(3) 0.39323(13) -0.05051(18) 0.0274(7) Uani 1 1 d . . . . .
H20 H 0.7237 0.3661 -0.0910 0.033 Uiso 1 1 calc R U . . .
C21 C 0.7167(3) 0.44685(13) -0.06983(18) 0.0310(7) Uani 1 1 d . . . . .
H21 H 0.6805 0.4564 -0.1232 0.037 Uiso 1 1 calc R U . . .
C22 C 0.7440(3) 0.48656(12) -0.01206(17) 0.0246(6) Uani 1 1 d . . . . .
H22 H 0.7273 0.5234 -0.0263 0.030 Uiso 1 1 calc R U . . .
C23 C 0.7961(3) 0.47364(11) 0.06743(16) 0.0202(6) Uani 1 1 d . . . . .
C24 C 0.8271(3) 0.31907(11) 0.04689(17) 0.0227(6) Uani 1 1 d . . . . .
H24 H 0.8177 0.3127 0.1054 0.027 Uiso 1 1 calc R U . . .
C25 C 0.9661(3) 0.30833(12) 0.0361(2) 0.0308(7) Uani 1 1 d . . . . .
H25A H 0.9806 0.3179 -0.0194 0.046 Uiso 1 1 calc R U . . .
H25B H 0.9854 0.2698 0.0458 0.046 Uiso 1 1 calc R U . . .
H25C H 1.0210 0.3304 0.0750 0.046 Uiso 1 1 calc R U . . .
C26 C 0.7412(3) 0.27838(13) -0.00340(19) 0.0339(7) Uani 1 1 d . . . . .
H26A H 0.6525 0.2872 0.0006 0.051 Uiso 1 1 calc R U . . .
H26B H 0.7595 0.2416 0.0174 0.051 Uiso 1 1 calc R U . . .
H26C H 0.7567 0.2803 -0.0604 0.051 Uiso 1 1 calc R U . . .
C27 C 0.8223(3) 0.51961(11) 0.12813(17) 0.0247(6) Uani 1 1 d . . . . .
H27 H 0.8686 0.5041 0.1791 0.030 Uiso 1 1 calc R U . . .
C28 C 0.6995(3) 0.54484(12) 0.1496(2) 0.0356(8) Uani 1 1 d . . . . .
H28A H 0.6457 0.5549 0.0996 0.053 Uiso 1 1 calc R U . . .
H28B H 0.7192 0.5773 0.1830 0.053 Uiso 1 1 calc R U . . .
H28C H 0.6550 0.5185 0.1801 0.053 Uiso 1 1 calc R U . . .
C29 C 0.9060(3) 0.56365(12) 0.0975(2) 0.0344(7) Uani 1 1 d . . . . .
H29A H 0.9821 0.5470 0.0807 0.052 Uiso 1 1 calc R U . . .
H29B H 0.9304 0.5898 0.1412 0.052 Uiso 1 1 calc R U . . .
H29C H 0.8591 0.5824 0.0511 0.052 Uiso 1 1 calc R U . . .
C30 C 0.7977(2) 0.49180(10) 0.37945(16) 0.0168(5) Uani 1 1 d . . . . .
C31 C 0.8414(3) 0.47058(11) 0.46511(16) 0.0201(6) Uani 1 1 d . . . . .
H31A H 0.7716 0.4512 0.4857 0.030 Uiso 1 1 calc R U . . .
H31B H 0.8675 0.5012 0.5011 0.030 Uiso 1 1 calc R U . . .
H31C H 0.9130 0.4458 0.4634 0.030 Uiso 1 1 calc R U . . .
C32 C 0.6858(3) 0.53084(11) 0.38203(18) 0.0230(6) Uani 1 1 d . . . . .
H32A H 0.6549 0.5428 0.3267 0.035 Uiso 1 1 calc R U . . .
H32B H 0.7134 0.5624 0.4155 0.035 Uiso 1 1 calc R U . . .
H32C H 0.6175 0.5122 0.4055 0.035 Uiso 1 1 calc R U . . .
C33 C 0.9077(3) 0.52194(11) 0.34756(17) 0.0217(6) Uani 1 1 d . . . . .
H33A H 0.9746 0.4960 0.3391 0.033 Uiso 1 1 calc R U . . .
H33B H 0.9414 0.5493 0.3873 0.033 Uiso 1 1 calc R U . . .
H33C H 0.8773 0.5397 0.2959 0.033 Uiso 1 1 calc R U . . .
C34 C 0.5299(3) 0.30124(11) 0.26983(17) 0.0215(6) Uani 1 1 d . . . . .
C35 C 0.5326(3) 0.25437(12) 0.33007(19) 0.0289(7) Uani 1 1 d . . . . .
H35A H 0.6205 0.2461 0.3513 0.043 Uiso 1 1 calc R U . . .
H35B H 0.4932 0.2223 0.3026 0.043 Uiso 1 1 calc R U . . .
H35C H 0.4858 0.2646 0.3751 0.043 Uiso 1 1 calc R U . . .
C36 C 0.3927(3) 0.31111(12) 0.23151(18) 0.0256(6) Uani 1 1 d . . . . .
H36A H 0.3410 0.3214 0.2740 0.038 Uiso 1 1 calc R U . . .
H36B H 0.3587 0.2778 0.2047 0.038 Uiso 1 1 calc R U . . .
H36C H 0.3910 0.3404 0.1914 0.038 Uiso 1 1 calc R U . . .
C37 C 0.6087(3) 0.28605(11) 0.20144(18) 0.0243(6) Uani 1 1 d . . . . .
H37A H 0.5980 0.3139 0.1590 0.036 Uiso 1 1 calc R U . . .
H37B H 0.5800 0.2510 0.1782 0.036 Uiso 1 1 calc R U . . .
H37C H 0.6982 0.2836 0.2236 0.036 Uiso 1 1 calc R U . . .
C38 C 0.4076(3) 0.44635(11) 0.31264(17) 0.0212(6) Uani 1 1 d . . . . .
H38A H 0.4680 0.4699 0.2882 0.025 Uiso 1 1 calc R U . . .
H38B H 0.3494 0.4303 0.2678 0.025 Uiso 1 1 calc R U . . .
C39 C 0.3307(3) 0.48134(11) 0.36541(17) 0.0235(6) Uani 1 1 d . . . . .
H39A H 0.2661 0.4582 0.3865 0.028 Uiso 1 1 calc R U . . .
H39B H 0.3880 0.4949 0.4127 0.028 Uiso 1 1 calc R U . . .
C40 C 0.2647(3) 0.52964(12) 0.32094(19) 0.0274(6) Uani 1 1 d . . . . .
H40A H 0.2065 0.5462 0.3561 0.033 Uiso 1 1 calc R U . . .
H40B H 0.2131 0.5164 0.2710 0.033 Uiso 1 1 calc R U . . .
C41 C 0.3557(3) 0.57319(12) 0.29755(19) 0.0301(7) Uani 1 1 d . . . . .
H41A H 0.4068 0.5868 0.3466 0.045 Uiso 1 1 calc R U . . .
H41B H 0.3073 0.6032 0.2702 0.045 Uiso 1 1 calc R U . . .
H41C H 0.4114 0.5576 0.2608 0.045 Uiso 1 1 calc R U . . .
C42 C 0.5206(3) 0.42284(15) 0.10862(19) 0.0327(7) Uani 1 1 d . . . . .
H42 H 0.5458 0.4422 0.0637 0.039 Uiso 1 1 calc R U . . .
N1 N 0.88470(19) 0.33726(8) 0.32172(12) 0.0126(4) Uani 1 1 d . . . . .
N2 N 0.86539(19) 0.40324(8) 0.16994(13) 0.0138(4) Uani 1 1 d . . . . .
N3 N 0.75898(19) 0.44560(8) 0.32661(13) 0.0139(4) Uani 1 1 d . . . . .
N4 N 0.5871(2) 0.35136(9) 0.31165(13) 0.0170(5) Uani 1 1 d . . . . .
O1 O 0.60814(18) 0.41601(8) 0.16874(12) 0.0248(4) Uani 1 1 d . . . . .
O2 O 0.4154(2) 0.40896(11) 0.10093(16) 0.0516(7) Uani 1 1 d . . . . .
Si1 Si 0.49720(7) 0.39056(3) 0.37068(5) 0.01795(16) Uani 1 1 d . . . . .
Nb1 Nb 0.73039(2) 0.38813(2) 0.26426(2) 0.01217(8) Uani 1 1 d . . . . .
H1A H 0.412(3) 0.3584(12) 0.4078(19) 0.030(8) Uiso 1 1 d . . . . .
H1B H 0.576(3) 0.4135(12) 0.4356(19) 0.030(8) Uiso 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.361(3) . ?
C1 C2 1.380(3) . ?
C1 C4 1.514(3) . ?
C2 C3 1.416(4) . ?
C2 H2 0.9500 . ?
C3 N2 1.325(3) . ?
C3 C5 1.514(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.408(4) . ?
C6 C11 1.408(4) . ?
C6 N1 1.465(3) . ?
C7 C8 1.395(4) . ?
C7 C12 1.524(4) . ?
C8 C9 1.380(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.381(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.392(4) . ?
C10 H10 0.9500 . ?
C11 C15 1.524(4) . ?
C12 C14 1.528(4) . ?
C12 C13 1.532(4) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.536(4) . ?
C15 C17 1.536(4) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.394(4) . ?
C18 C23 1.407(4) . ?
C18 N2 1.460(3) . ?
C19 C20 1.400(4) . ?
C19 C24 1.522(4) . ?
C20 C21 1.378(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.375(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.402(4) . ?
C22 H22 0.9500 . ?
C23 C27 1.518(4) . ?
C24 C26 1.532(4) . ?
C24 C25 1.536(4) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.530(4) . ?
C27 C29 1.530(4) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N3 1.464(3) . ?
C30 C31 1.531(4) . ?
C30 C33 1.535(3) . ?
C30 C32 1.537(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 N4 1.508(3) . ?
C34 C35 1.524(4) . ?
C34 C37 1.538(4) . ?
C34 C36 1.539(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.535(4) . ?
C38 Si1 1.870(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.525(4) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.528(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 O2 1.163(4) . ?
C42 O1 1.289(3) . ?
C42 H42 0.9500 . ?
N1 Nb1 2.189(2) . ?
N2 Nb1 2.282(2) . ?
N3 Nb1 1.757(2) . ?
N4 Si1 1.743(2) . ?
N4 Nb1 2.016(2) . ?
O1 Nb1 2.0406(19) . ?
Si1 H1A 1.40(3) . ?
Si1 H1B 1.40(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 124.5(2) . . ?
N1 C1 C4 120.4(2) . . ?
C2 C1 C4 115.1(2) . . ?
C1 C2 C3 129.7(2) . . ?
C1 C2 H2 115.2 . . ?
C3 C2 H2 115.2 . . ?
N2 C3 C2 123.2(2) . . ?
N2 C3 C5 121.8(2) . . ?
C2 C3 C5 114.9(2) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 119.9(2) . . ?
C7 C6 N1 121.8(2) . . ?
C11 C6 N1 118.2(2) . . ?
C8 C7 C6 118.8(2) . . ?
C8 C7 C12 117.3(2) . . ?
C6 C7 C12 123.9(2) . . ?
C9 C8 C7 121.8(3) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C8 C9 C10 118.9(3) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C9 C10 C11 121.8(3) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C10 C11 C6 118.8(3) . . ?
C10 C11 C15 118.3(2) . . ?
C6 C11 C15 122.8(2) . . ?
C7 C12 C14 111.5(2) . . ?
C7 C12 C13 111.6(2) . . ?
C14 C12 C13 107.9(2) . . ?
C7 C12 H12 108.6 . . ?
C14 C12 H12 108.6 . . ?
C13 C12 H12 108.6 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C16 110.2(2) . . ?
C11 C15 C17 112.5(2) . . ?
C16 C15 C17 109.8(2) . . ?
C11 C15 H15 108.1 . . ?
C16 C15 H15 108.1 . . ?
C17 C15 H15 108.1 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 121.3(3) . . ?
C19 C18 N2 119.1(2) . . ?
C23 C18 N2 119.5(2) . . ?
C18 C19 C20 118.5(3) . . ?
C18 C19 C24 121.4(2) . . ?
C20 C19 C24 120.0(3) . . ?
C21 C20 C19 120.9(3) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C22 C21 C20 120.1(3) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C23 121.2(3) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 H22 119.4 . . ?
C22 C23 C18 117.9(3) . . ?
C22 C23 C27 118.2(2) . . ?
C18 C23 C27 123.9(2) . . ?
C19 C24 C26 113.9(2) . . ?
C19 C24 C25 110.2(2) . . ?
C26 C24 C25 110.1(2) . . ?
C19 C24 H24 107.5 . . ?
C26 C24 H24 107.5 . . ?
C25 C24 H24 107.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 C28 111.4(3) . . ?
C23 C27 C29 112.1(2) . . ?
C28 C27 C29 109.8(2) . . ?
C23 C27 H27 107.8 . . ?
C28 C27 H27 107.8 . . ?
C29 C27 H27 107.8 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C31 108.7(2) . . ?
N3 C30 C33 109.9(2) . . ?
C31 C30 C33 109.1(2) . . ?
N3 C30 C32 110.0(2) . . ?
C31 C30 C32 109.6(2) . . ?
C33 C30 C32 109.5(2) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N4 C34 C35 110.2(2) . . ?
N4 C34 C37 108.2(2) . . ?
C35 C34 C37 109.3(2) . . ?
N4 C34 C36 111.7(2) . . ?
C35 C34 C36 109.3(2) . . ?
C37 C34 C36 108.1(2) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 Si1 113.19(19) . . ?
C39 C38 H38A 108.9 . . ?
Si1 C38 H38A 108.9 . . ?
C39 C38 H38B 108.9 . . ?
Si1 C38 H38B 108.9 . . ?
H38A C38 H38B 107.8 . . ?
C40 C39 C38 114.2(2) . . ?
C40 C39 H39A 108.7 . . ?
C38 C39 H39A 108.7 . . ?
C40 C39 H39B 108.7 . . ?
C38 C39 H39B 108.7 . . ?
H39A C39 H39B 107.6 . . ?
C39 C40 C41 113.7(2) . . ?
C39 C40 H40A 108.8 . . ?
C41 C40 H40A 108.8 . . ?
C39 C40 H40B 108.8 . . ?
C41 C40 H40B 108.8 . . ?
H40A C40 H40B 107.7 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O2 C42 O1 129.9(3) . . ?
O2 C42 H42 115.1 . . ?
O1 C42 H42 115.1 . . ?
C1 N1 C6 114.4(2) . . ?
C1 N1 Nb1 117.70(16) . . ?
C6 N1 Nb1 127.71(16) . . ?
C3 N2 C18 117.6(2) . . ?
C3 N2 Nb1 119.33(17) . . ?
C18 N2 Nb1 121.63(15) . . ?
C30 N3 Nb1 173.62(18) . . ?
C34 N4 Si1 119.54(17) . . ?
C34 N4 Nb1 118.12(16) . . ?
Si1 N4 Nb1 117.69(11) . . ?
C42 O1 Nb1 167.2(2) . . ?
N4 Si1 C38 113.53(11) . . ?
N4 Si1 H1A 111.3(12) . . ?
C38 Si1 H1A 108.9(13) . . ?
N4 Si1 H1B 109.6(13) . . ?
C38 Si1 H1B 108.5(13) . . ?
H1A Si1 H1B 104.5(18) . . ?
N3 Nb1 N4 102.55(9) . . ?
N3 Nb1 O1 103.47(9) . . ?
N4 Nb1 O1 90.72(8) . . ?
N3 Nb1 N1 98.00(9) . . ?
N4 Nb1 N1 97.86(8) . . ?
O1 Nb1 N1 154.55(8) . . ?
N3 Nb1 N2 101.17(8) . . ?
N4 Nb1 N2 155.78(8) . . ?
O1 Nb1 N2 78.99(8) . . ?
N1 Nb1 N2 83.62(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -13.4(4) . . . . ?
C4 C1 C2 C3 166.8(3) . . . . ?
C1 C2 C3 N2 20.3(4) . . . . ?
C1 C2 C3 C5 -160.0(3) . . . . ?
C11 C6 C7 C8 0.4(4) . . . . ?
N1 C6 C7 C8 -176.1(2) . . . . ?
C11 C6 C7 C12 178.5(2) . . . . ?
N1 C6 C7 C12 2.0(4) . . . . ?
C6 C7 C8 C9 -0.3(4) . . . . ?
C12 C7 C8 C9 -178.5(3) . . . . ?
C7 C8 C9 C10 0.2(5) . . . . ?
C8 C9 C10 C11 -0.1(5) . . . . ?
C9 C10 C11 C6 0.2(4) . . . . ?
C9 C10 C11 C15 176.7(3) . . . . ?
C7 C6 C11 C10 -0.3(4) . . . . ?
N1 C6 C11 C10 176.3(2) . . . . ?
C7 C6 C11 C15 -176.7(3) . . . . ?
N1 C6 C11 C15 -0.1(4) . . . . ?
C8 C7 C12 C14 -52.6(3) . . . . ?
C6 C7 C12 C14 129.2(3) . . . . ?
C8 C7 C12 C13 68.1(3) . . . . ?
C6 C7 C12 C13 -110.1(3) . . . . ?
C10 C11 C15 C16 -76.1(3) . . . . ?
C6 C11 C15 C16 100.3(3) . . . . ?
C10 C11 C15 C17 46.8(4) . . . . ?
C6 C11 C15 C17 -136.8(3) . . . . ?
C23 C18 C19 C20 -1.1(4) . . . . ?
N2 C18 C19 C20 176.1(2) . . . . ?
C23 C18 C19 C24 175.6(2) . . . . ?
N2 C18 C19 C24 -7.2(4) . . . . ?
C18 C19 C20 C21 0.1(4) . . . . ?
C24 C19 C20 C21 -176.7(3) . . . . ?
C19 C20 C21 C22 0.9(5) . . . . ?
C20 C21 C22 C23 -0.8(5) . . . . ?
C21 C22 C23 C18 -0.3(4) . . . . ?
C21 C22 C23 C27 -179.3(3) . . . . ?
C19 C18 C23 C22 1.2(4) . . . . ?
N2 C18 C23 C22 -175.9(2) . . . . ?
C19 C18 C23 C27 -179.7(2) . . . . ?
N2 C18 C23 C27 3.1(4) . . . . ?
C18 C19 C24 C26 151.8(3) . . . . ?
C20 C19 C24 C26 -31.6(4) . . . . ?
C18 C19 C24 C25 -84.0(3) . . . . ?
C20 C19 C24 C25 92.7(3) . . . . ?
C22 C23 C27 C28 68.9(3) . . . . ?
C18 C23 C27 C28 -110.2(3) . . . . ?
C22 C23 C27 C29 -54.7(3) . . . . ?
C18 C23 C27 C29 126.3(3) . . . . ?
Si1 C38 C39 C40 175.7(2) . . . . ?
C38 C39 C40 C41 -67.9(3) . . . . ?
C2 C1 N1 C6 155.2(2) . . . . ?
C4 C1 N1 C6 -25.0(3) . . . . ?
C2 C1 N1 Nb1 -29.6(3) . . . . ?
C4 C1 N1 Nb1 150.22(18) . . . . ?
C7 C6 N1 C1 96.7(3) . . . . ?
C11 C6 N1 C1 -79.8(3) . . . . ?
C7 C6 N1 Nb1 -77.9(3) . . . . ?
C11 C6 N1 Nb1 105.5(2) . . . . ?
C2 C3 N2 C18 -176.9(2) . . . . ?
C5 C3 N2 C18 3.4(3) . . . . ?
C2 C3 N2 Nb1 16.6(3) . . . . ?
C5 C3 N2 Nb1 -163.04(18) . . . . ?
C19 C18 N2 C3 102.5(3) . . . . ?
C23 C18 N2 C3 -80.3(3) . . . . ?
C19 C18 N2 Nb1 -91.4(2) . . . . ?
C23 C18 N2 Nb1 85.8(3) . . . . ?
C35 C34 N4 Si1 -79.3(3) . . . . ?
C37 C34 N4 Si1 161.21(19) . . . . ?
C36 C34 N4 Si1 42.3(3) . . . . ?
C35 C34 N4 Nb1 125.4(2) . . . . ?
C37 C34 N4 Nb1 5.9(3) . . . . ?
C36 C34 N4 Nb1 -113.0(2) . . . . ?
O2 C42 O1 Nb1 42.3(12) . . . . ?
C34 N4 Si1 C38 -91.2(2) . . . . ?
Nb1 N4 Si1 C38 64.19(16) . . . . ?
C39 C38 Si1 N4 -178.89(18) . . . . ?

_refine_diff_density_max         0.630
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.072


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-pentane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bmkxr54
_database_code_depnum_ccdc_archive 'CCDC 2004314'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-17 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_audit_creation_date             2020-05-16
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            (BDI)Nb(OC(H)O)(N[BO2C6H12]tBu)(NtBu)
_chemical_name_systematic        
Formato-(N-(tert-butyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-amino)-(tert-butyl)imino-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V)
_chemical_formula_moiety         'C44 H72 B N4 Nb O4'
_chemical_formula_sum            'C44 H72 B N4 Nb O4'
_chemical_formula_weight         824.77
_chemical_absolute_configuration ?
_chemical_melting_point          386
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P 1 n 1'
_space_group_name_Hall           'P -2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, z+1/2'

_cell_length_a                   12.5350(5)
_cell_length_b                   17.4460(8)
_cell_length_c                   20.5667(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.552(2)
_cell_angle_gamma                90
_cell_volume                     4468.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.31
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.969
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0906 before and 0.0538 after correction.
The Ratio of minimum to maximum transmission is 0.9718.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_number            8187
_diffrn_reflns_point_group_measured_fraction_full 0.500
_diffrn_reflns_point_group_measured_fraction_max 0.499
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.392
_diffrn_reflns_theta_min         1.167
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                6977
_reflns_number_total             8187
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.08(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1013
_refine_ls_number_reflns         8187
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0384
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0313P)²+3.2854P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0847
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C56(H56), C59(H59), C68(H68), C71(H71)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C44(H44),
 C46(H46), C52(H52), C53(H53), C54(H54), C64(H64), C65(H65), C66(H66), C88(H88)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C57(H57A,
 H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C),
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C73(H73A,H73B,
 H73C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C79(H79A,
 H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C84(H84A,H84B,H84C),
 C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6379(5) 1.0273(3) 0.3996(2) 0.0248(14) Uani 1 1 d . . . . .
C2 C 0.5353(5) 1.0432(4) 0.4148(3) 0.0238(14) Uani 1 1 d . . . . .
H2 H 0.514259 1.095505 0.411755 0.029 Uiso 1 1 calc R . . . .
C3 C 0.4580(5) 0.9918(4) 0.4343(3) 0.0227(14) Uani 1 1 d . . . . .
C4 C 0.6910(5) 1.0923(3) 0.3657(3) 0.0310(14) Uani 1 1 d . . . . .
H4A H 0.740049 1.120157 0.397944 0.046 Uiso 1 1 calc GR . . . .
H4B H 0.635719 1.127465 0.345681 0.046 Uiso 1 1 calc GR . . . .
H4C H 0.731328 1.071172 0.331761 0.046 Uiso 1 1 calc GR . . . .
C5 C 0.3425(5) 1.0218(3) 0.4198(3) 0.0256(14) Uani 1 1 d . . . . .
H5A H 0.320275 1.019440 0.372553 0.038 Uiso 1 1 calc GR . . . .
H5B H 0.339265 1.074963 0.434737 0.038 Uiso 1 1 calc GR . . . .
H5C H 0.294306 0.990040 0.442758 0.038 Uiso 1 1 calc GR . . . .
C6 C 0.7764(5) 0.9445(3) 0.3727(3) 0.0301(14) Uani 1 1 d . . . . .
C7 C 0.8810(5) 0.9611(4) 0.3953(3) 0.0362(15) Uani 1 1 d . . . . .
C8 C 0.9604(6) 0.9503(4) 0.3521(4) 0.0440(19) Uani 1 1 d . . . . .
H8 H 1.033326 0.962395 0.366103 0.053 Uiso 1 1 calc R . . . .
C9 C 0.9319(7) 0.9221(4) 0.2900(3) 0.052(2) Uani 1 1 d . . . . .
H9 H 0.985448 0.915330 0.261331 0.062 Uiso 1 1 calc R . . . .
C10 C 0.8275(7) 0.9039(4) 0.2689(3) 0.0473(19) Uani 1 1 d . . . . .
H10 H 0.810115 0.882998 0.226344 0.057 Uiso 1 1 calc R . . . .
C11 C 0.7474(6) 0.9153(4) 0.3082(3) 0.0360(16) Uani 1 1 d . . . . .
C12 C 0.9162(5) 0.9925(4) 0.4623(4) 0.0359(18) Uani 1 1 d . . . . .
H12 H 0.853369 0.990680 0.488216 0.043 Uiso 1 1 calc R . . . .
C13 C 1.0067(5) 0.9445(5) 0.4983(4) 0.054(2) Uani 1 1 d . . . . .
H13A H 0.984265 0.890688 0.498981 0.081 Uiso 1 1 calc GR . . . .
H13B H 1.022516 0.963182 0.543316 0.081 Uiso 1 1 calc GR . . . .
H13C H 1.071088 0.948811 0.475693 0.081 Uiso 1 1 calc GR . . . .
C14 C 0.9555(6) 1.0758(4) 0.4614(4) 0.054(2) Uani 1 1 d . . . . .
H14A H 1.022398 1.078007 0.441013 0.081 Uiso 1 1 calc GR . . . .
H14B H 0.968399 1.095223 0.506340 0.081 Uiso 1 1 calc GR . . . .
H14C H 0.900847 1.107457 0.436267 0.081 Uiso 1 1 calc GR . . . .
C15 C 0.6330(6) 0.8979(4) 0.2814(3) 0.0410(17) Uani 1 1 d . . . . .
H15 H 0.589949 0.893610 0.319290 0.049 Uiso 1 1 calc R . . . .
C16 C 0.6191(6) 0.8226(4) 0.2424(3) 0.054(2) Uani 1 1 d . . . . .
H16A H 0.649177 0.828485 0.200757 0.080 Uiso 1 1 calc GR . . . .
H16B H 0.542524 0.810087 0.233847 0.080 Uiso 1 1 calc GR . . . .
H16C H 0.656664 0.781134 0.267767 0.080 Uiso 1 1 calc GR . . . .
C17 C 0.5860(6) 0.9638(4) 0.2380(3) 0.055(2) Uani 1 1 d . . . . .
H17A H 0.586151 1.010830 0.264074 0.083 Uiso 1 1 calc GR . . . .
H17B H 0.512137 0.951285 0.220261 0.083 Uiso 1 1 calc GR . . . .
H17C H 0.629586 0.971493 0.201906 0.083 Uiso 1 1 calc GR . . . .
C18 C 0.3876(5) 0.8759(3) 0.4707(3) 0.0257(13) Uani 1 1 d . . . . .
C19 C 0.3417(5) 0.8292(4) 0.4206(3) 0.0367(16) Uani 1 1 d . . . . .
C20 C 0.2451(6) 0.7890(4) 0.4311(4) 0.045(2) Uani 1 1 d . . . . .
H20 H 0.210635 0.757673 0.397224 0.054 Uiso 1 1 calc R . . . .
C21 C 0.2025(5) 0.7948(4) 0.4879(4) 0.0505(19) Uani 1 1 d . . . . .
H21 H 0.137918 0.768455 0.493503 0.061 Uiso 1 1 calc R . . . .
C22 C 0.2518(5) 0.8385(4) 0.5377(4) 0.0453(18) Uani 1 1 d . . . . .
H22 H 0.221266 0.840736 0.577839 0.054 Uiso 1 1 calc R . . . .
C23 C 0.3460(6) 0.8803(4) 0.5317(3) 0.0297(17) Uani 1 1 d . . . . .
C24 C 0.3896(6) 0.8191(4) 0.3572(3) 0.0380(19) Uani 1 1 d . . . . .
H24 H 0.464331 0.840141 0.363327 0.046 Uiso 1 1 calc R . . . .
C25 C 0.3963(6) 0.7339(4) 0.3382(3) 0.050(2) Uani 1 1 d . . . . .
H25A H 0.426111 0.704125 0.376415 0.074 Uiso 1 1 calc GR . . . .
H25B H 0.442721 0.728420 0.303214 0.074 Uiso 1 1 calc GR . . . .
H25C H 0.324219 0.714873 0.322797 0.074 Uiso 1 1 calc GR . . . .
C26 C 0.3257(7) 0.8636(4) 0.3006(3) 0.062(2) Uani 1 1 d . . . . .
H26A H 0.359799 0.856564 0.260426 0.093 Uiso 1 1 calc GR . . . .
H26B H 0.324768 0.918239 0.311541 0.093 Uiso 1 1 calc GR . . . .
H26C H 0.251868 0.844182 0.293827 0.093 Uiso 1 1 calc GR . . . .
C27 C 0.3917(5) 0.9295(4) 0.5882(3) 0.0315(14) Uani 1 1 d . . . . .
H27 H 0.469081 0.939057 0.583419 0.038 Uiso 1 1 calc R . . . .
C28 C 0.3353(5) 1.0076(4) 0.5891(3) 0.0433(18) Uani 1 1 d . . . . .
H28A H 0.347315 1.036566 0.549793 0.065 Uiso 1 1 calc GR . . . .
H28B H 0.364612 1.036284 0.628100 0.065 Uiso 1 1 calc GR . . . .
H28C H 0.258122 0.999745 0.590093 0.065 Uiso 1 1 calc GR . . . .
C29 C 0.3859(5) 0.8901(4) 0.6544(3) 0.0472(18) Uani 1 1 d . . . . .
H29A H 0.312167 0.892739 0.665831 0.071 Uiso 1 1 calc GR . . . .
H29B H 0.434288 0.916154 0.688197 0.071 Uiso 1 1 calc GR . . . .
H29C H 0.407477 0.836374 0.651528 0.071 Uiso 1 1 calc GR . . . .
C30 C 0.6982(4) 1.0171(3) 0.6079(3) 0.0267(13) Uani 1 1 d . . . . .
C31 C 0.6208(5) 1.0837(4) 0.5885(3) 0.0365(15) Uani 1 1 d . . . . .
H31A H 0.636288 1.105097 0.546523 0.055 Uiso 1 1 calc GR . . . .
H31B H 0.630038 1.123671 0.622195 0.055 Uiso 1 1 calc GR . . . .
H31C H 0.546653 1.064925 0.584424 0.055 Uiso 1 1 calc GR . . . .
C32 C 0.8140(5) 1.0463(4) 0.6119(3) 0.0393(16) Uani 1 1 d . . . . .
H32A H 0.863682 1.002932 0.619074 0.059 Uiso 1 1 calc GR . . . .
H32B H 0.827396 1.082576 0.648293 0.059 Uiso 1 1 calc GR . . . .
H32C H 0.825174 1.072044 0.570853 0.059 Uiso 1 1 calc GR . . . .
C33 C 0.6780(6) 0.9831(4) 0.6736(3) 0.0407(18) Uani 1 1 d . . . . .
H33A H 0.604390 0.963500 0.670709 0.061 Uiso 1 1 calc GR . . . .
H33B H 0.688111 1.022805 0.707421 0.061 Uiso 1 1 calc GR . . . .
H33C H 0.728667 0.941072 0.684848 0.061 Uiso 1 1 calc GR . . . .
C34 C 0.7649(5) 0.7478(3) 0.4586(3) 0.0263(14) Uani 1 1 d . . . . .
C35 C 0.8629(5) 0.7436(4) 0.4214(3) 0.0351(15) Uani 1 1 d . . . . .
H35A H 0.868849 0.791224 0.396748 0.053 Uiso 1 1 calc GR . . . .
H35B H 0.855376 0.700178 0.390971 0.053 Uiso 1 1 calc GR . . . .
H35C H 0.927540 0.736779 0.452394 0.053 Uiso 1 1 calc GR . . . .
C36 C 0.7468(5) 0.6709(3) 0.4918(3) 0.0298(14) Uani 1 1 d . . . . .
H36A H 0.811574 0.656953 0.520738 0.045 Uiso 1 1 calc GR . . . .
H36B H 0.731420 0.631130 0.458424 0.045 Uiso 1 1 calc GR . . . .
H36C H 0.686043 0.675438 0.517615 0.045 Uiso 1 1 calc GR . . . .
C37 C 0.6635(5) 0.7629(4) 0.4109(3) 0.0329(15) Uani 1 1 d . . . . .
H37A H 0.600384 0.762537 0.434951 0.049 Uiso 1 1 calc GR . . . .
H37B H 0.656025 0.722803 0.377309 0.049 Uiso 1 1 calc GR . . . .
H37C H 0.669544 0.812959 0.390045 0.049 Uiso 1 1 calc GR . . . .
C38 C 0.9442(4) 0.8181(3) 0.6658(3) 0.0254(13) Uani 1 1 d . . . . .
C39 C 0.9552(5) 0.7358(4) 0.6417(3) 0.0245(13) Uani 1 1 d . . . . .
C40 C 0.9129(5) 0.8271(4) 0.7339(3) 0.0308(14) Uani 1 1 d . . . . .
H40A H 0.910781 0.881657 0.744957 0.046 Uiso 1 1 calc GR . . . .
H40B H 0.965737 0.801020 0.765168 0.046 Uiso 1 1 calc GR . . . .
H40C H 0.841871 0.804384 0.736025 0.046 Uiso 1 1 calc GR . . . .
C41 C 1.0430(5) 0.8667(4) 0.6577(3) 0.0329(15) Uani 1 1 d . . . . .
H41A H 1.066397 0.857047 0.614592 0.049 Uiso 1 1 calc GR . . . .
H41B H 1.100992 0.853291 0.691869 0.049 Uiso 1 1 calc GR . . . .
H41C H 1.025052 0.921108 0.661467 0.049 Uiso 1 1 calc GR . . . .
C42 C 1.0679(4) 0.7013(4) 0.6540(3) 0.0328(14) Uani 1 1 d . . . . .
H42A H 1.066422 0.648391 0.638015 0.049 Uiso 1 1 calc GR . . . .
H42B H 1.091902 0.701907 0.701073 0.049 Uiso 1 1 calc GR . . . .
H42C H 1.117517 0.731612 0.630888 0.049 Uiso 1 1 calc GR . . . .
C43 C 0.8744(4) 0.6800(3) 0.6661(3) 0.0273(13) Uani 1 1 d . . . . .
H43A H 0.801759 0.700886 0.656489 0.041 Uiso 1 1 calc GR . . . .
H43B H 0.890986 0.672844 0.713389 0.041 Uiso 1 1 calc GR . . . .
H43C H 0.878794 0.630587 0.643873 0.041 Uiso 1 1 calc GR . . . .
C44 C 0.5861(5) 0.7842(4) 0.6013(3) 0.0274(13) Uani 1 1 d . . . . .
H44 H 0.628075 0.816127 0.631629 0.033 Uiso 1 1 calc R . . . .
C45 C 0.3559(4) 0.5438(3) 0.5879(2) 0.0187(12) Uani 1 1 d . . . . .
C46 C 0.4656(4) 0.5445(3) 0.5860(3) 0.0166(12) Uani 1 1 d . . . . .
H46 H 0.495863 0.593783 0.580917 0.020 Uiso 1 1 calc R . . . .
C47 C 0.5389(5) 0.4840(4) 0.5902(3) 0.0176(13) Uani 1 1 d . . . . .
C48 C 0.3101(4) 0.6201(3) 0.6065(3) 0.0262(13) Uani 1 1 d . . . . .
H48A H 0.231906 0.615974 0.605000 0.039 Uiso 1 1 calc GR . . . .
H48B H 0.327913 0.659616 0.575555 0.039 Uiso 1 1 calc GR . . . .
H48C H 0.340895 0.634182 0.650804 0.039 Uiso 1 1 calc GR . . . .
C49 C 0.6537(5) 0.5057(3) 0.6153(3) 0.0236(14) Uani 1 1 d . . . . .
H49A H 0.665971 0.496793 0.662648 0.035 Uiso 1 1 calc GR . . . .
H49B H 0.665592 0.559917 0.606164 0.035 Uiso 1 1 calc GR . . . .
H49C H 0.703568 0.474193 0.593367 0.035 Uiso 1 1 calc GR . . . .
C50 C 0.1851(4) 0.4838(3) 0.5976(2) 0.0188(11) Uani 1 1 d . . . . .
C51 C 0.0961(5) 0.4971(3) 0.5508(3) 0.0192(13) Uani 1 1 d . . . . .
C52 C -0.0055(5) 0.4960(3) 0.5719(3) 0.0276(13) Uani 1 1 d . . . . .
H52 H -0.066346 0.505938 0.541108 0.033 Uiso 1 1 calc R . . . .
C53 C -0.0211(5) 0.4809(3) 0.6357(3) 0.0280(13) Uani 1 1 d . . . . .
H53 H -0.091625 0.477642 0.648132 0.034 Uiso 1 1 calc R . . . .
C54 C 0.0671(5) 0.4707(4) 0.6815(3) 0.0269(14) Uani 1 1 d . . . . .
H54 H 0.056702 0.461747 0.725950 0.032 Uiso 1 1 calc R . . . .
C55 C 0.1721(4) 0.4733(3) 0.6636(2) 0.0205(12) Uani 1 1 d . . . . .
C56 C 0.1073(4) 0.5159(3) 0.4801(3) 0.0235(12) Uani 1 1 d . . . . .
H56 H 0.172987 0.489568 0.467792 0.028 Uiso 1 1 calc R . . . .
C57 C 0.0113(5) 0.4888(4) 0.4335(3) 0.0341(15) Uani 1 1 d . . . . .
H57A H -0.005223 0.435439 0.443518 0.051 Uiso 1 1 calc GR . . . .
H57B H 0.028382 0.492316 0.388298 0.051 Uiso 1 1 calc GR . . . .
H57C H -0.051059 0.521118 0.438845 0.051 Uiso 1 1 calc GR . . . .
C58 C 0.1208(5) 0.6020(4) 0.4704(3) 0.0393(16) Uani 1 1 d . . . . .
H58A H 0.063259 0.629535 0.489046 0.059 Uiso 1 1 calc GR . . . .
H58B H 0.117327 0.613398 0.423556 0.059 Uiso 1 1 calc GR . . . .
H58C H 0.190509 0.618442 0.492465 0.059 Uiso 1 1 calc GR . . . .
C59 C 0.2637(5) 0.4685(3) 0.7197(3) 0.0277(13) Uani 1 1 d . . . . .
H59 H 0.333308 0.466239 0.700397 0.033 Uiso 1 1 calc R . . . .
C60 C 0.2648(5) 0.5388(4) 0.7631(3) 0.0403(16) Uani 1 1 d . . . . .
H60A H 0.274393 0.584754 0.736976 0.060 Uiso 1 1 calc GR . . . .
H60B H 0.324041 0.534758 0.798328 0.060 Uiso 1 1 calc GR . . . .
H60C H 0.196572 0.542248 0.781906 0.060 Uiso 1 1 calc GR . . . .
C61 C 0.2553(6) 0.3972(4) 0.7628(3) 0.0378(16) Uani 1 1 d . . . . .
H61A H 0.188438 0.399384 0.783284 0.057 Uiso 1 1 calc GR . . . .
H61B H 0.316606 0.395732 0.796932 0.057 Uiso 1 1 calc GR . . . .
H61C H 0.255409 0.350938 0.735773 0.057 Uiso 1 1 calc GR . . . .
C62 C 0.5964(4) 0.3554(3) 0.5967(2) 0.0182(11) Uani 1 1 d . . . . .
C63 C 0.6070(5) 0.3261(4) 0.6607(3) 0.0243(15) Uani 1 1 d . . . . .
C64 C 0.6980(5) 0.2835(3) 0.6818(3) 0.0321(14) Uani 1 1 d . . . . .
H64 H 0.706262 0.263254 0.724929 0.039 Uiso 1 1 calc R . . . .
C65 C 0.7758(5) 0.2702(3) 0.6417(3) 0.0324(14) Uani 1 1 d . . . . .
H65 H 0.840049 0.244371 0.658133 0.039 Uiso 1 1 calc R . . . .
C66 C 0.7610(5) 0.2940(4) 0.5783(3) 0.0296(16) Uani 1 1 d . . . . .
H66 H 0.813391 0.281076 0.550197 0.036 Uiso 1 1 calc R . . . .
C67 C 0.6713(4) 0.3368(3) 0.5532(3) 0.0220(12) Uani 1 1 d . . . . .
C68 C 0.5235(4) 0.3391(3) 0.7074(2) 0.0251(13) Uani 1 1 d . . . . .
H68 H 0.459078 0.362792 0.682086 0.030 Uiso 1 1 calc R . . . .
C69 C 0.4887(5) 0.2637(4) 0.7355(3) 0.0353(15) Uani 1 1 d . . . . .
H69A H 0.472087 0.226689 0.699958 0.053 Uiso 1 1 calc GR . . . .
H69B H 0.424702 0.272229 0.757811 0.053 Uiso 1 1 calc GR . . . .
H69C H 0.546840 0.243713 0.766779 0.053 Uiso 1 1 calc GR . . . .
C70 C 0.5634(5) 0.3940(4) 0.7630(3) 0.0389(16) Uani 1 1 d . . . . .
H70A H 0.509323 0.397970 0.793641 0.058 Uiso 1 1 calc GR . . . .
H70B H 0.575905 0.444701 0.744811 0.058 Uiso 1 1 calc GR . . . .
H70C H 0.630675 0.374428 0.786057 0.058 Uiso 1 1 calc GR . . . .
C71 C 0.6601(5) 0.3601(4) 0.4829(3) 0.0281(16) Uani 1 1 d . . . . .
H71 H 0.586024 0.380979 0.471568 0.034 Uiso 1 1 calc R . . . .
C72 C 0.7404(5) 0.4224(4) 0.4676(3) 0.0341(15) Uani 1 1 d . . . . .
H72A H 0.728165 0.468863 0.492446 0.051 Uiso 1 1 calc GR . . . .
H72B H 0.730369 0.433943 0.420658 0.051 Uiso 1 1 calc GR . . . .
H72C H 0.813810 0.404035 0.479925 0.051 Uiso 1 1 calc GR . . . .
C73 C 0.6734(5) 0.2910(4) 0.4377(3) 0.0390(16) Uani 1 1 d . . . . .
H73A H 0.748933 0.275209 0.442071 0.059 Uiso 1 1 calc GR . . . .
H73B H 0.650652 0.305488 0.392182 0.059 Uiso 1 1 calc GR . . . .
H73C H 0.629093 0.248281 0.450091 0.059 Uiso 1 1 calc GR . . . .
C74 C 0.4022(4) 0.4777(3) 0.3910(2) 0.0239(12) Uani 1 1 d . . . . .
C75 C 0.4449(5) 0.4200(4) 0.3446(3) 0.0355(15) Uani 1 1 d . . . . .
H75A H 0.514084 0.399822 0.364343 0.053 Uiso 1 1 calc GR . . . .
H75B H 0.454441 0.445303 0.303081 0.053 Uiso 1 1 calc GR . . . .
H75C H 0.393618 0.377710 0.336412 0.053 Uiso 1 1 calc GR . . . .
C76 C 0.4887(4) 0.5373(3) 0.4136(3) 0.0285(14) Uani 1 1 d . . . . .
H76A H 0.457843 0.576790 0.439677 0.043 Uiso 1 1 calc GR . . . .
H76B H 0.514979 0.560967 0.375257 0.043 Uiso 1 1 calc GR . . . .
H76C H 0.548391 0.512052 0.440221 0.043 Uiso 1 1 calc GR . . . .
C77 C 0.3019(5) 0.5173(4) 0.3569(3) 0.0337(16) Uani 1 1 d . . . . .
H77A H 0.245777 0.478976 0.345181 0.050 Uiso 1 1 calc GR . . . .
H77B H 0.319791 0.542952 0.317144 0.050 Uiso 1 1 calc GR . . . .
H77C H 0.275889 0.555246 0.386474 0.050 Uiso 1 1 calc GR . . . .
C78 C 0.1887(4) 0.2713(3) 0.5488(2) 0.0175(12) Uani 1 1 d . . . . .
C79 C 0.0709(4) 0.2836(3) 0.5606(3) 0.0243(12) Uani 1 1 d . . . . .
H79A H 0.058963 0.337982 0.569357 0.036 Uiso 1 1 calc GR . . . .
H79B H 0.055017 0.253010 0.598299 0.036 Uiso 1 1 calc GR . . . .
H79C H 0.023623 0.267705 0.521699 0.036 Uiso 1 1 calc GR . . . .
C80 C 0.2622(4) 0.2915(3) 0.6116(2) 0.0231(12) Uani 1 1 d . . . . .
H80A H 0.336485 0.277710 0.606189 0.035 Uiso 1 1 calc GR . . . .
H80B H 0.239106 0.263091 0.648653 0.035 Uiso 1 1 calc GR . . . .
H80C H 0.257980 0.346680 0.620025 0.035 Uiso 1 1 calc GR . . . .
C81 C 0.2071(5) 0.1865(3) 0.5352(3) 0.0244(13) Uani 1 1 d . . . . .
H81A H 0.161459 0.171085 0.495475 0.037 Uiso 1 1 calc GR . . . .
H81B H 0.188930 0.155802 0.572285 0.037 Uiso 1 1 calc GR . . . .
H81C H 0.282624 0.178326 0.529090 0.037 Uiso 1 1 calc GR . . . .
C82 C 0.1130(4) 0.3209(3) 0.3204(3) 0.0243(13) Uani 1 1 d . . . . .
C83 C 0.0466(5) 0.2565(4) 0.3477(3) 0.0303(15) Uani 1 1 d . . . . .
C84 C 0.2045(6) 0.2904(5) 0.2870(3) 0.058(2) Uani 1 1 d . . . . .
H84A H 0.251342 0.332795 0.277173 0.087 Uiso 1 1 calc GR . . . .
H84B H 0.176238 0.264862 0.246144 0.087 Uiso 1 1 calc GR . . . .
H84C H 0.245677 0.253490 0.315733 0.087 Uiso 1 1 calc GR . . . .
C85 C 0.0508(6) 0.3774(4) 0.2754(3) 0.050(2) Uani 1 1 d . . . . .
H85A H -0.007200 0.399646 0.297544 0.074 Uiso 1 1 calc GR . . . .
H85B H 0.020099 0.351101 0.235523 0.074 Uiso 1 1 calc GR . . . .
H85C H 0.098928 0.418286 0.263995 0.074 Uiso 1 1 calc GR . . . .
C86 C -0.0698(5) 0.2810(5) 0.3538(3) 0.053(2) Uani 1 1 d . . . . .
H86A H -0.103006 0.243987 0.381166 0.079 Uiso 1 1 calc GR . . . .
H86B H -0.110483 0.282679 0.310240 0.079 Uiso 1 1 calc GR . . . .
H86C H -0.069906 0.331909 0.373949 0.079 Uiso 1 1 calc GR . . . .
C87 C 0.0450(7) 0.1817(4) 0.3110(3) 0.057(2) Uani 1 1 d . . . . .
H87A H 0.115591 0.157194 0.319085 0.086 Uiso 1 1 calc GR . . . .
H87B H 0.027949 0.191421 0.264044 0.086 Uiso 1 1 calc GR . . . .
H87C H -0.009611 0.147918 0.326052 0.086 Uiso 1 1 calc GR . . . .
C88 C 0.4351(4) 0.2309(3) 0.4698(3) 0.0256(13) Uani 1 1 d . . . . .
H88 H 0.471458 0.185061 0.484146 0.031 Uiso 1 1 calc R . . . .
N1 N 0.6889(4) 0.9599(3) 0.4125(2) 0.0218(11) Uani 1 1 d . . . . .
N2 N 0.4800(4) 0.9231(3) 0.4596(2) 0.0195(11) Uani 1 1 d . . . . .
N3 N 0.6820(4) 0.9572(3) 0.5578(2) 0.0195(10) Uani 1 1 d . . . . .
N4 N 0.7768(4) 0.8144(3) 0.5068(2) 0.0206(11) Uani 1 1 d . . . . .
N5 N 0.2937(3) 0.4810(3) 0.5771(2) 0.0161(10) Uani 1 1 d . . . . .
N6 N 0.5113(3) 0.4109(3) 0.5777(2) 0.0172(10) Uani 1 1 d . . . . .
N7 N 0.3730(3) 0.4365(3) 0.4483(2) 0.0196(10) Uani 1 1 d . . . . .
N8 N 0.2154(4) 0.3229(3) 0.4954(2) 0.0162(11) Uani 1 1 d . . . . .
O1 O 0.8565(3) 0.8480(2) 0.61947(18) 0.0225(9) Uani 1 1 d . . . . .
O2 O 0.9269(3) 0.7443(2) 0.57140(17) 0.0230(9) Uani 1 1 d . . . . .
O3 O 0.5662(3) 0.8095(2) 0.54210(17) 0.0221(8) Uani 1 1 d . . . . .
O4 O 0.5567(4) 0.7244(3) 0.6216(2) 0.0437(12) Uani 1 1 d . . . . .
O5 O 0.1623(3) 0.3593(2) 0.37911(17) 0.0236(10) Uani 1 1 d . . . . .
O6 O 0.0961(3) 0.2476(2) 0.41422(18) 0.0312(10) Uani 1 1 d . . . . .
O7 O 0.4374(3) 0.2851(2) 0.51286(17) 0.0209(8) Uani 1 1 d . . . . .
O8 O 0.3933(3) 0.2305(3) 0.4142(2) 0.0367(11) Uani 1 1 d . . . . .
Nb1 Nb 0.65226(3) 0.88986(3) 0.49561(2) 0.01646(13) Uani 1 1 d . . . . .
Nb2 Nb 0.35205(3) 0.38625(3) 0.51814(2) 0.01379(12) Uani 1 1 d . . . . .
B1 B 0.8528(5) 0.8034(4) 0.5636(3) 0.0192(15) Uani 1 1 d . . . . .
B2 B 0.1604(5) 0.3101(4) 0.4304(3) 0.0185(15) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.386(9) . ?
C1 C4 1.524(8) . ?
C1 N1 1.350(7) . ?
C2 H2 0.9500 . ?
C2 C3 1.411(9) . ?
C3 C5 1.536(8) . ?
C3 N2 1.324(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.372(9) . ?
C6 C11 1.427(8) . ?
C6 N1 1.467(7) . ?
C7 C8 1.421(9) . ?
C7 C12 1.501(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.378(10) . ?
C9 H9 0.9500 . ?
C9 C10 1.368(11) . ?
C10 H10 0.9500 . ?
C10 C11 1.374(9) . ?
C11 C15 1.508(10) . ?
C12 H12 1.0000 . ?
C12 C13 1.531(9) . ?
C12 C14 1.536(10) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.538(9) . ?
C15 C17 1.532(9) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.386(8) . ?
C18 C23 1.415(9) . ?
C18 N2 1.459(7) . ?
C19 C20 1.437(10) . ?
C19 C24 1.507(10) . ?
C20 H20 0.9500 . ?
C20 C21 1.341(11) . ?
C21 H21 0.9500 . ?
C21 C22 1.366(10) . ?
C22 H22 0.9500 . ?
C22 C23 1.405(9) . ?
C23 C27 1.506(9) . ?
C24 H24 1.0000 . ?
C24 C25 1.543(9) . ?
C24 C26 1.546(9) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27 1.0000 . ?
C27 C28 1.535(9) . ?
C27 C29 1.534(8) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.537(8) . ?
C30 C32 1.532(8) . ?
C30 C33 1.522(8) . ?
C30 N3 1.466(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.522(8) . ?
C34 C36 1.534(8) . ?
C34 C37 1.536(8) . ?
C34 N4 1.525(7) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.531(8) . ?
C38 C40 1.505(8) . ?
C38 C41 1.526(8) . ?
C38 O1 1.466(6) . ?
C39 C42 1.529(8) . ?
C39 C43 1.529(8) . ?
C39 O2 1.457(6) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44 0.9500 . ?
C44 O3 1.292(6) . ?
C44 O4 1.197(7) . ?
C45 C46 1.380(8) . ?
C45 C48 1.516(7) . ?
C45 N5 1.348(7) . ?
C46 H46 0.9500 . ?
C46 C47 1.395(8) . ?
C47 C49 1.520(8) . ?
C47 N6 1.339(7) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.408(8) . ?
C50 C55 1.397(7) . ?
C50 N5 1.471(7) . ?
C51 C52 1.392(8) . ?
C51 C56 1.513(8) . ?
C52 H52 0.9500 . ?
C52 C53 1.373(8) . ?
C53 H53 0.9500 . ?
C53 C54 1.379(8) . ?
C54 H54 0.9500 . ?
C54 C55 1.408(8) . ?
C55 C59 1.534(7) . ?
C56 H56 1.0000 . ?
C56 C57 1.525(7) . ?
C56 C58 1.528(8) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59 1.0000 . ?
C59 C60 1.515(8) . ?
C59 C61 1.540(8) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C63 1.403(8) . ?
C62 C67 1.408(7) . ?
C62 N6 1.461(7) . ?
C63 C64 1.388(8) . ?
C63 C68 1.516(8) . ?
C64 H64 0.9500 . ?
C64 C65 1.367(8) . ?
C65 H65 0.9500 . ?
C65 C66 1.361(9) . ?
C66 H66 0.9500 . ?
C66 C67 1.399(8) . ?
C67 C71 1.493(9) . ?
C68 H68 1.0000 . ?
C68 C69 1.519(8) . ?
C68 C70 1.531(7) . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 H71 1.0000 . ?
C71 C72 1.538(9) . ?
C71 C73 1.543(8) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 C75 1.527(8) . ?
C74 C76 1.534(8) . ?
C74 C77 1.533(8) . ?
C74 N7 1.462(7) . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 C79 1.538(7) . ?
C78 C80 1.540(7) . ?
C78 C81 1.527(8) . ?
C78 N8 1.488(7) . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 C83 1.541(8) . ?
C82 C84 1.501(9) . ?
C82 C85 1.508(8) . ?
C82 O5 1.455(6) . ?
C83 C86 1.539(9) . ?
C83 C87 1.507(9) . ?
C83 O6 1.445(6) . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C88 H88 0.9500 . ?
C88 O7 1.294(6) . ?
C88 O8 1.204(7) . ?
N1 Nb1 2.192(4) . ?
N2 Nb1 2.276(4) . ?
N3 Nb1 1.746(4) . ?
N4 Nb1 2.035(5) . ?
N4 B1 1.433(8) . ?
N5 Nb2 2.222(4) . ?
N6 Nb2 2.261(4) . ?
N7 Nb2 1.728(4) . ?
N8 Nb2 2.047(4) . ?
N8 B2 1.450(8) . ?
O1 B1 1.383(7) . ?
O2 B1 1.385(8) . ?
O3 Nb1 2.069(4) . ?
O5 B2 1.362(8) . ?
O6 B2 1.374(8) . ?
O7 Nb2 2.072(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C4 114.8(5) . . ?
N1 C1 C2 124.1(6) . . ?
N1 C1 C4 121.1(5) . . ?
C1 C2 H2 115.8 . . ?
C1 C2 C3 128.4(6) . . ?
C3 C2 H2 115.8 . . ?
C2 C3 C5 113.0(5) . . ?
N2 C3 C2 124.6(6) . . ?
N2 C3 C5 122.3(6) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 121.6(6) . . ?
C7 C6 N1 121.2(5) . . ?
C11 C6 N1 117.2(5) . . ?
C6 C7 C8 118.0(6) . . ?
C6 C7 C12 123.9(6) . . ?
C8 C7 C12 118.0(6) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.1(7) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 119.5 . . ?
C10 C9 C8 121.0(6) . . ?
C10 C9 H9 119.5 . . ?
C9 C10 H10 119.5 . . ?
C9 C10 C11 121.1(7) . . ?
C11 C10 H10 119.5 . . ?
C6 C11 C15 122.9(5) . . ?
C10 C11 C6 118.2(7) . . ?
C10 C11 C15 118.9(6) . . ?
C7 C12 H12 108.1 . . ?
C7 C12 C13 111.6(6) . . ?
C7 C12 C14 113.2(6) . . ?
C13 C12 H12 108.1 . . ?
C13 C12 C14 107.6(6) . . ?
C14 C12 H12 108.1 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15 107.7 . . ?
C11 C15 C16 114.2(6) . . ?
C11 C15 C17 110.4(6) . . ?
C16 C15 H15 107.7 . . ?
C17 C15 H15 107.7 . . ?
C17 C15 C16 109.0(5) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 121.7(6) . . ?
C19 C18 N2 119.1(5) . . ?
C23 C18 N2 119.2(5) . . ?
C18 C19 C20 117.5(7) . . ?
C18 C19 C24 122.6(6) . . ?
C20 C19 C24 120.0(6) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 C19 121.3(7) . . ?
C21 C20 H20 119.4 . . ?
C20 C21 H21 119.9 . . ?
C20 C21 C22 120.3(7) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 118.8 . . ?
C21 C22 C23 122.4(7) . . ?
C23 C22 H22 118.8 . . ?
C18 C23 C27 124.7(6) . . ?
C22 C23 C18 116.7(6) . . ?
C22 C23 C27 118.5(6) . . ?
C19 C24 H24 108.0 . . ?
C19 C24 C25 111.7(6) . . ?
C19 C24 C26 111.7(6) . . ?
C25 C24 H24 108.0 . . ?
C25 C24 C26 109.3(5) . . ?
C26 C24 H24 108.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27 107.9 . . ?
C23 C27 C28 112.4(5) . . ?
C23 C27 C29 112.2(6) . . ?
C28 C27 H27 107.9 . . ?
C29 C27 H27 107.9 . . ?
C29 C27 C28 108.5(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C32 C30 C31 109.2(5) . . ?
C33 C30 C31 111.2(5) . . ?
C33 C30 C32 109.5(5) . . ?
N3 C30 C31 108.9(4) . . ?
N3 C30 C32 109.2(5) . . ?
N3 C30 C33 108.8(5) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C36 110.6(5) . . ?
C35 C34 C37 110.1(5) . . ?
C35 C34 N4 109.8(5) . . ?
C36 C34 C37 106.4(5) . . ?
N4 C34 C36 112.7(4) . . ?
N4 C34 C37 107.3(5) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C40 C38 C39 116.2(5) . . ?
C40 C38 C41 110.2(5) . . ?
C41 C38 C39 112.5(5) . . ?
O1 C38 C39 102.2(4) . . ?
O1 C38 C40 108.2(5) . . ?
O1 C38 C41 106.8(4) . . ?
C42 C39 C38 115.5(5) . . ?
C42 C39 C43 109.2(5) . . ?
C43 C39 C38 113.8(5) . . ?
O2 C39 C38 101.8(4) . . ?
O2 C39 C42 108.7(4) . . ?
O2 C39 C43 107.1(5) . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C39 C43 H43A 109.5 . . ?
C39 C43 H43B 109.5 . . ?
C39 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O3 C44 H44 116.8 . . ?
O4 C44 H44 116.8 . . ?
O4 C44 O3 126.3(6) . . ?
C46 C45 C48 114.0(5) . . ?
N5 C45 C46 124.2(5) . . ?
N5 C45 C48 121.8(5) . . ?
C45 C46 H46 115.0 . . ?
C45 C46 C47 130.0(6) . . ?
C47 C46 H46 115.0 . . ?
C46 C47 C49 115.1(5) . . ?
N6 C47 C46 123.6(5) . . ?
N6 C47 C49 121.1(5) . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 N5 119.7(5) . . ?
C55 C50 C51 120.9(5) . . ?
C55 C50 N5 119.3(4) . . ?
C50 C51 C56 122.7(5) . . ?
C52 C51 C50 117.8(5) . . ?
C52 C51 C56 119.5(5) . . ?
C51 C52 H52 118.8 . . ?
C53 C52 C51 122.4(5) . . ?
C53 C52 H52 118.8 . . ?
C52 C53 H53 120.4 . . ?
C52 C53 C54 119.2(5) . . ?
C54 C53 H53 120.4 . . ?
C53 C54 H54 119.5 . . ?
C53 C54 C55 121.1(5) . . ?
C55 C54 H54 119.5 . . ?
C50 C55 C54 118.4(5) . . ?
C50 C55 C59 125.2(5) . . ?
C54 C55 C59 116.3(5) . . ?
C51 C56 H56 108.2 . . ?
C51 C56 C57 112.5(5) . . ?
C51 C56 C58 111.2(5) . . ?
C57 C56 H56 108.2 . . ?
C57 C56 C58 108.4(5) . . ?
C58 C56 H56 108.2 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C55 C59 H59 108.4 . . ?
C55 C59 C61 112.5(5) . . ?
C60 C59 C55 110.8(5) . . ?
C60 C59 H59 108.4 . . ?
C60 C59 C61 108.1(5) . . ?
C61 C59 H59 108.4 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C63 C62 C67 120.9(5) . . ?
C63 C62 N6 118.7(5) . . ?
C67 C62 N6 120.1(5) . . ?
C62 C63 C68 122.8(5) . . ?
C64 C63 C62 118.3(6) . . ?
C64 C63 C68 118.9(5) . . ?
C63 C64 H64 119.3 . . ?
C65 C64 C63 121.4(6) . . ?
C65 C64 H64 119.3 . . ?
C64 C65 H65 120.1 . . ?
C66 C65 C64 119.8(5) . . ?
C66 C65 H65 120.1 . . ?
C65 C66 H66 118.9 . . ?
C65 C66 C67 122.2(6) . . ?
C67 C66 H66 118.9 . . ?
C62 C67 C71 123.9(5) . . ?
C66 C67 C62 117.0(5) . . ?
C66 C67 C71 119.1(5) . . ?
C63 C68 H68 107.8 . . ?
C63 C68 C69 111.2(5) . . ?
C63 C68 C70 112.1(5) . . ?
C69 C68 H68 107.8 . . ?
C69 C68 C70 110.0(5) . . ?
C70 C68 H68 107.8 . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C68 C70 H70A 109.5 . . ?
C68 C70 H70B 109.5 . . ?
C68 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C67 C71 H71 107.8 . . ?
C67 C71 C72 113.5(5) . . ?
C67 C71 C73 111.5(6) . . ?
C72 C71 H71 107.8 . . ?
C72 C71 C73 108.1(5) . . ?
C73 C71 H71 107.8 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72B 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C75 C74 C76 110.5(5) . . ?
C75 C74 C77 109.8(5) . . ?
C77 C74 C76 110.3(5) . . ?
N7 C74 C75 108.6(5) . . ?
N7 C74 C76 108.8(4) . . ?
N7 C74 C77 108.8(4) . . ?
C74 C75 H75A 109.5 . . ?
C74 C75 H75B 109.5 . . ?
C74 C75 H75C 109.5 . . ?
H75A C75 H75B 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C74 C76 H76A 109.5 . . ?
C74 C76 H76B 109.5 . . ?
C74 C76 H76C 109.5 . . ?
H76A C76 H76B 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C74 C77 H77A 109.5 . . ?
C74 C77 H77B 109.5 . . ?
C74 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C79 C78 C80 109.2(4) . . ?
C81 C78 C79 109.4(4) . . ?
C81 C78 C80 106.7(4) . . ?
N8 C78 C79 109.4(4) . . ?
N8 C78 C80 108.5(4) . . ?
N8 C78 C81 113.5(4) . . ?
C78 C79 H79A 109.5 . . ?
C78 C79 H79B 109.5 . . ?
C78 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C78 C80 H80A 109.5 . . ?
C78 C80 H80B 109.5 . . ?
C78 C80 H80C 109.5 . . ?
H80A C80 H80B 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C78 C81 H81A 109.5 . . ?
C78 C81 H81B 109.5 . . ?
C78 C81 H81C 109.5 . . ?
H81A C81 H81B 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C84 C82 C83 112.4(6) . . ?
C84 C82 C85 108.7(6) . . ?
C85 C82 C83 115.9(5) . . ?
O5 C82 C83 103.3(4) . . ?
O5 C82 C84 105.6(4) . . ?
O5 C82 C85 110.4(5) . . ?
C86 C83 C82 112.6(6) . . ?
C87 C83 C82 115.2(5) . . ?
C87 C83 C86 108.8(6) . . ?
O6 C83 C82 103.4(4) . . ?
O6 C83 C86 105.2(5) . . ?
O6 C83 C87 111.2(5) . . ?
C82 C84 H84A 109.5 . . ?
C82 C84 H84B 109.5 . . ?
C82 C84 H84C 109.5 . . ?
H84A C84 H84B 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C82 C85 H85A 109.5 . . ?
C82 C85 H85B 109.5 . . ?
C82 C85 H85C 109.5 . . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C83 C86 H86A 109.5 . . ?
C83 C86 H86B 109.5 . . ?
C83 C86 H86C 109.5 . . ?
H86A C86 H86B 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C83 C87 H87A 109.5 . . ?
C83 C87 H87B 109.5 . . ?
C83 C87 H87C 109.5 . . ?
H87A C87 H87B 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
O7 C88 H88 115.6 . . ?
O8 C88 H88 115.6 . . ?
O8 C88 O7 128.9(6) . . ?
C1 N1 C6 114.7(4) . . ?
C1 N1 Nb1 120.1(4) . . ?
C6 N1 Nb1 124.8(3) . . ?
C3 N2 C18 116.0(5) . . ?
C3 N2 Nb1 120.4(4) . . ?
C18 N2 Nb1 123.1(3) . . ?
C30 N3 Nb1 175.0(4) . . ?
C34 N4 Nb1 113.7(3) . . ?
B1 N4 C34 115.8(5) . . ?
B1 N4 Nb1 127.5(4) . . ?
C45 N5 C50 117.5(4) . . ?
C45 N5 Nb2 118.3(3) . . ?
C50 N5 Nb2 123.7(3) . . ?
C47 N6 C62 114.6(4) . . ?
C47 N6 Nb2 118.6(4) . . ?
C62 N6 Nb2 126.2(3) . . ?
C74 N7 Nb2 174.2(4) . . ?
C78 N8 Nb2 114.3(3) . . ?
B2 N8 C78 117.6(5) . . ?
B2 N8 Nb2 126.2(4) . . ?
B1 O1 C38 107.0(5) . . ?
B1 O2 C39 105.9(4) . . ?
C44 O3 Nb1 127.8(3) . . ?
B2 O5 C82 108.0(5) . . ?
B2 O6 C83 108.7(5) . . ?
C88 O7 Nb2 133.4(3) . . ?
N1 Nb1 N2 83.11(17) . . ?
N3 Nb1 N1 98.60(19) . . ?
N3 Nb1 N2 100.51(18) . . ?
N3 Nb1 N4 104.8(2) . . ?
N3 Nb1 O3 101.36(18) . . ?
N4 Nb1 N1 102.86(18) . . ?
N4 Nb1 N2 152.70(18) . . ?
N4 Nb1 O3 86.71(17) . . ?
O3 Nb1 N1 154.84(16) . . ?
O3 Nb1 N2 78.34(15) . . ?
N5 Nb2 N6 83.58(16) . . ?
N7 Nb2 N5 99.55(19) . . ?
N7 Nb2 N6 98.33(18) . . ?
N7 Nb2 N8 106.66(19) . . ?
N7 Nb2 O7 105.09(18) . . ?
N8 Nb2 N5 101.96(17) . . ?
N8 Nb2 N6 152.94(17) . . ?
N8 Nb2 O7 87.26(17) . . ?
O7 Nb2 N5 149.98(15) . . ?
O7 Nb2 N6 76.19(15) . . ?
O1 B1 N4 123.9(6) . . ?
O1 B1 O2 111.3(5) . . ?
O2 B1 N4 124.6(5) . . ?
O5 B2 N8 124.6(6) . . ?
O5 B2 O6 112.0(5) . . ?
O6 B2 N8 123.3(5) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexamethyldisiloxane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bmkxr40
_database_code_depnum_ccdc_archive 'CCDC 2004315'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-17 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_audit_creation_date             2020-05-17
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            (BDI)Nb(NtBu)(NHtBu)(CCtBu)
_chemical_name_systematic        
(3,3-diemethylbut-1-ynylyl)-(tert-butyl)amino-(tert-butyl)imino-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V)
_chemical_formula_moiety         'C43 H69 N4 Nb'
_chemical_formula_sum            'C43 H69 N4 Nb'
_chemical_formula_weight         734.93
_chemical_melting_point          463
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.517(2)
_cell_length_b                   18.7959(18)
_cell_length_c                   22.580(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8283.2(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9375
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.35
_shelx_estimated_absorpt_T_max   0.975
_shelx_estimated_absorpt_T_min   0.962
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0977 before and 0.0696 after correction.
The Ratio of minimum to maximum transmission is 0.9528.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_number            7601
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.407
_diffrn_reflns_theta_min         1.754
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6392
_reflns_number_total             7601
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.028
_refine_diff_density_min         -1.251
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         7601
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0447
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0168P)²+22.5747P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0970
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N4) = Uanis(Nb1)
3.a Ternary CH refined with riding coordinates:
 C27(H27), C12(H12), C24(H24), C15(H15)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C21(H21), C22(H22), C8(H8), C9(H9), C10(H10), C20(H20)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C41(H41A,H41B,H41C), C35(H35A,H35B,H35C), C28(H28A,H28B,
 H28C), C36(H36A,H36B,H36C), C4(H4A,H4B,H4C), C29(H29A,H29B,H29C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C), C31(H31A,H31B,H31C), C37(H37A,H37B,H37C),
 C13(H13A,H13B,H13C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C16(H16A,
 H16B,H16C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.82754(2) 0.12933(2) 0.06631(2) 0.01667(8) Uani 1 1 d . . . . .
N2 N 0.72085(12) 0.15651(12) 0.04374(10) 0.0188(5) Uani 1 1 d . . . . .
N3 N 0.87486(12) 0.20292(13) 0.03795(11) 0.0235(5) Uani 1 1 d . . . . .
N4 N 0.84111(11) 0.05935(12) 0.00297(10) 0.01667(8) Uani 1 1 d . . . . .
N1 N 0.79797(12) 0.17479(12) 0.15694(10) 0.0202(5) Uani 1 1 d . . . . .
C27 C 0.62063(15) 0.05389(16) 0.08493(13) 0.0246(6) Uani 1 1 d . . . . .
H27 H 0.663081 0.067268 0.107086 0.029 Uiso 1 1 calc R . . . .
C23 C 0.63396(13) 0.06649(15) 0.01937(13) 0.0195(6) Uani 1 1 d . . . . .
C18 C 0.68150(14) 0.11749(15) -0.00042(12) 0.0196(6) Uani 1 1 d . . . . .
C2 C 0.71586(15) 0.25516(16) 0.11242(13) 0.0238(6) Uani 1 1 d . . . . .
H2 H 0.701277 0.303286 0.114907 0.029 Uiso 1 1 calc R . . . .
C5 C 0.63530(16) 0.25257(17) 0.02955(14) 0.0301(7) Uani 1 1 d . . . . .
H5A H 0.653551 0.283130 -0.001883 0.045 Uiso 1 1 calc GR . . . .
H5B H 0.607900 0.281264 0.056970 0.045 Uiso 1 1 calc GR . . . .
H5C H 0.606447 0.215466 0.012008 0.045 Uiso 1 1 calc GR . . . .
C39 C 0.92700(17) 0.02109(16) 0.15027(13) 0.0275(7) Uani 1 1 d . . . . .
C7 C 0.88845(16) 0.18244(16) 0.23359(13) 0.0249(7) Uani 1 1 d . . . . .
C34 C 0.83412(15) -0.01758(15) -0.00461(13) 0.0233(6) Uani 1 1 d . . . . .
C40 C 0.96368(16) -0.03460(16) 0.18420(13) 0.0266(7) Uani 1 1 d . . . . .
C6 C 0.82645(15) 0.15308(15) 0.21369(12) 0.0213(6) Uani 1 1 d . . . . .
C11 C 0.78978(16) 0.10475(18) 0.24863(13) 0.0295(7) Uani 1 1 d . . . . .
C21 C 0.60287(15) 0.04225(17) -0.08267(13) 0.0277(7) Uani 1 1 d . . . . .
H21 H 0.576162 0.016643 -0.110649 0.033 Uiso 1 1 calc R . . . .
C1 C 0.75674(15) 0.23099(16) 0.15970(13) 0.0241(6) Uani 1 1 d . . . . .
C12 C 0.93324(17) 0.22898(16) 0.19462(14) 0.0308(7) Uani 1 1 d . . . . .
H12 H 0.916151 0.224271 0.153050 0.037 Uiso 1 1 calc R . . . .
C19 C 0.68898(14) 0.13105(16) -0.06146(13) 0.0253(7) Uani 1 1 d . . . . .
C41 C 0.96664(19) -0.01356(18) 0.24960(14) 0.0379(8) Uani 1 1 d . . . . .
H41A H 0.990289 0.032190 0.253590 0.057 Uiso 1 1 calc GR . . . .
H41B H 0.991565 -0.050057 0.271884 0.057 Uiso 1 1 calc GR . . . .
H41C H 0.919974 -0.009322 0.265222 0.057 Uiso 1 1 calc GR . . . .
C22 C 0.59576(14) 0.02889(16) -0.02272(13) 0.0242(6) Uani 1 1 d . . . . .
H22 H 0.564340 -0.006494 -0.009878 0.029 Uiso 1 1 calc R . . . .
C3 C 0.69404(14) 0.21835(15) 0.06283(12) 0.0207(6) Uani 1 1 d . . . . .
C38 C 0.89629(18) 0.06599(16) 0.12257(13) 0.0308(7) Uani 1 1 d . . . . .
C35 C 0.79147(16) -0.04632(17) 0.04673(15) 0.0337(8) Uani 1 1 d . . . . .
H35A H 0.815337 -0.037133 0.084144 0.051 Uiso 1 1 calc GR . . . .
H35B H 0.784941 -0.097676 0.041800 0.051 Uiso 1 1 calc GR . . . .
H35C H 0.746756 -0.022611 0.047222 0.051 Uiso 1 1 calc GR . . . .
C8 C 0.90887(17) 0.16795(17) 0.29163(13) 0.0299(7) Uani 1 1 d . . . . .
H8 H 0.949827 0.188706 0.306410 0.036 Uiso 1 1 calc R . . . .
C9 C 0.87096(17) 0.12428(19) 0.32781(13) 0.0347(8) Uani 1 1 d . . . . .
H9 H 0.884780 0.116714 0.367653 0.042 Uiso 1 1 calc R . . . .
C10 C 0.81298(17) 0.09150(19) 0.30636(14) 0.0350(8) Uani 1 1 d . . . . .
H10 H 0.788354 0.059485 0.330997 0.042 Uiso 1 1 calc R . . . .
C28 C 0.60332(16) -0.02332(17) 0.10056(15) 0.0320(7) Uani 1 1 d . . . . .
H28A H 0.559408 -0.036317 0.082502 0.048 Uiso 1 1 calc GR . . . .
H28B H 0.600099 -0.028287 0.143669 0.048 Uiso 1 1 calc GR . . . .
H28C H 0.639383 -0.054768 0.085495 0.048 Uiso 1 1 calc GR . . . .
C36 C 0.90603(15) -0.05041(18) -0.00413(14) 0.0315(7) Uani 1 1 d . . . . .
H36A H 0.932793 -0.031085 -0.037143 0.047 Uiso 1 1 calc GR . . . .
H36B H 0.902424 -0.102177 -0.008297 0.047 Uiso 1 1 calc GR . . . .
H36C H 0.928825 -0.038967 0.033343 0.047 Uiso 1 1 calc GR . . . .
C30 C 0.91292(16) 0.25733(17) 0.00715(13) 0.0287(7) Uani 1 1 d . . . . .
C24 C 0.73782(17) 0.18679(18) -0.08679(14) 0.0348(8) Uani 1 1 d . . . . .
H24 H 0.763717 0.208656 -0.053195 0.042 Uiso 1 1 calc R . . . .
C4 C 0.74644(19) 0.27254(19) 0.21658(14) 0.0384(9) Uani 1 1 d . . . . .
H4A H 0.706684 0.253576 0.237886 0.058 Uiso 1 1 calc GR . . . .
H4B H 0.738604 0.322783 0.207176 0.058 Uiso 1 1 calc GR . . . .
H4C H 0.787375 0.268105 0.241447 0.058 Uiso 1 1 calc GR . . . .
C29 C 0.56229(19) 0.10218(19) 0.10664(16) 0.0419(9) Uani 1 1 d . . . . .
H29A H 0.575874 0.152106 0.102285 0.063 Uiso 1 1 calc GR . . . .
H29B H 0.552755 0.092084 0.148409 0.063 Uiso 1 1 calc GR . . . .
H29C H 0.521039 0.093165 0.083059 0.063 Uiso 1 1 calc GR . . . .
C15 C 0.72629(17) 0.0668(2) 0.22635(15) 0.0420(9) Uani 1 1 d . . . . .
H15 H 0.722497 0.076992 0.183007 0.050 Uiso 1 1 calc R . . . .
C25 C 0.6987(2) 0.24638(19) -0.11932(15) 0.0411(9) Uani 1 1 d . . . . .
H25A H 0.674666 0.226309 -0.153579 0.062 Uiso 1 1 calc GR . . . .
H25B H 0.731160 0.282720 -0.132751 0.062 Uiso 1 1 calc GR . . . .
H25C H 0.665342 0.267978 -0.092301 0.062 Uiso 1 1 calc GR . . . .
C20 C 0.64876(16) 0.09275(18) -0.10140(14) 0.0301(7) Uani 1 1 d . . . . .
H20 H 0.653266 0.101888 -0.142598 0.036 Uiso 1 1 calc R . . . .
C26 C 0.78967(17) 0.1540(2) -0.12990(15) 0.0401(9) Uani 1 1 d . . . . .
H26A H 0.816143 0.117121 -0.109465 0.060 Uiso 1 1 calc GR . . . .
H26B H 0.820756 0.191109 -0.144309 0.060 Uiso 1 1 calc GR . . . .
H26C H 0.765248 0.132824 -0.163475 0.060 Uiso 1 1 calc GR . . . .
C31 C 0.96906(17) 0.28694(18) 0.04775(14) 0.0335(8) Uani 1 1 d . . . . .
H31A H 0.948045 0.307575 0.083226 0.050 Uiso 1 1 calc GR . . . .
H31B H 0.994905 0.323753 0.026647 0.050 Uiso 1 1 calc GR . . . .
H31C H 1.000118 0.248399 0.059331 0.050 Uiso 1 1 calc GR . . . .
C37 C 0.79816(18) -0.0342(2) -0.06295(16) 0.0417(9) Uani 1 1 d . . . . .
H37A H 0.751982 -0.013739 -0.062465 0.063 Uiso 1 1 calc GR . . . .
H37B H 0.795058 -0.085874 -0.068060 0.063 Uiso 1 1 calc GR . . . .
H37C H 0.824342 -0.013667 -0.095802 0.063 Uiso 1 1 calc GR . . . .
C13 C 1.00732(18) 0.2047(2) 0.19531(18) 0.0458(9) Uani 1 1 d . . . . .
H13A H 1.025896 0.209763 0.235415 0.069 Uiso 1 1 calc GR . . . .
H13B H 1.034102 0.234023 0.167851 0.069 Uiso 1 1 calc GR . . . .
H13C H 1.009864 0.154777 0.183108 0.069 Uiso 1 1 calc GR . . . .
C42 C 0.92631(19) -0.10573(17) 0.17712(17) 0.0406(9) Uani 1 1 d . . . . .
H42A H 0.880039 -0.101799 0.193654 0.061 Uiso 1 1 calc GR . . . .
H42B H 0.951609 -0.142995 0.198169 0.061 Uiso 1 1 calc GR . . . .
H42C H 0.923361 -0.117914 0.134995 0.061 Uiso 1 1 calc GR . . . .
C43 C 1.03679(18) -0.04202(19) 0.15969(16) 0.0400(8) Uani 1 1 d . . . . .
H43A H 1.034796 -0.057945 0.118402 0.060 Uiso 1 1 calc GR . . . .
H43B H 1.062135 -0.076954 0.183319 0.060 Uiso 1 1 calc GR . . . .
H43C H 1.060076 0.004113 0.161727 0.060 Uiso 1 1 calc GR . . . .
C32 C 0.8612(2) 0.3179(2) -0.0076(2) 0.0538(11) Uani 1 1 d . . . . .
H32A H 0.828867 0.301352 -0.037790 0.081 Uiso 1 1 calc GR . . . .
H32B H 0.886150 0.359445 -0.022517 0.081 Uiso 1 1 calc GR . . . .
H32C H 0.835984 0.331091 0.028334 0.081 Uiso 1 1 calc GR . . . .
C33 C 0.9435(2) 0.2282(2) -0.04871(17) 0.0558(12) Uani 1 1 d . . . . .
H33A H 0.969635 0.184991 -0.039601 0.084 Uiso 1 1 calc GR . . . .
H33B H 0.974145 0.263752 -0.066239 0.084 Uiso 1 1 calc GR . . . .
H33C H 0.906881 0.216736 -0.076787 0.084 Uiso 1 1 calc GR . . . .
C14 C 0.9285(2) 0.30771(19) 0.2117(2) 0.0573(12) Uani 1 1 d . . . . .
H14A H 0.936317 0.312885 0.254315 0.086 Uiso 1 1 calc GR . . . .
H14B H 0.882813 0.325829 0.201701 0.086 Uiso 1 1 calc GR . . . .
H14C H 0.963203 0.334779 0.189888 0.086 Uiso 1 1 calc GR . . . .
C17 C 0.6618(2) 0.0949(3) 0.2554(3) 0.0798(16) Uani 1 1 d . . . . .
H17A H 0.621956 0.069026 0.240115 0.120 Uiso 1 1 calc GR . . . .
H17B H 0.656807 0.145715 0.246492 0.120 Uiso 1 1 calc GR . . . .
H17C H 0.664839 0.088290 0.298356 0.120 Uiso 1 1 calc GR . . . .
C16 C 0.7318(2) -0.0122(2) 0.2332(2) 0.0674(13) Uani 1 1 d . . . . .
H16A H 0.734654 -0.024308 0.275321 0.101 Uiso 1 1 calc GR . . . .
H16B H 0.773008 -0.029213 0.212812 0.101 Uiso 1 1 calc GR . . . .
H16C H 0.691271 -0.034956 0.215836 0.101 Uiso 1 1 calc GR . . . .
H4 H 0.8684(18) 0.0736(18) -0.0299(16) 0.042(10) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 N2 2.204(2) . ?
Nb1 N3 1.782(2) . ?
Nb1 N4 1.961(2) . ?
Nb1 N1 2.291(2) . ?
Nb1 C38 2.198(3) . ?
N2 C18 1.457(3) . ?
N2 C3 1.346(4) . ?
N3 C30 1.443(4) . ?
N4 C34 1.462(4) . ?
N4 H4 0.95(4) . ?
N1 C6 1.455(3) . ?
N1 C1 1.329(4) . ?
C27 H27 1.0000 . ?
C27 C23 1.522(4) . ?
C27 C28 1.531(4) . ?
C27 C29 1.536(4) . ?
C23 C18 1.407(4) . ?
C23 C22 1.399(4) . ?
C18 C19 1.409(4) . ?
C2 H2 0.9500 . ?
C2 C1 1.408(4) . ?
C2 C3 1.383(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C5 C3 1.514(4) . ?
C39 C40 1.482(4) . ?
C39 C38 1.209(4) . ?
C7 C6 1.404(4) . ?
C7 C12 1.518(4) . ?
C7 C8 1.397(4) . ?
C34 C35 1.526(4) . ?
C34 C36 1.533(4) . ?
C34 C37 1.525(4) . ?
C40 C41 1.530(4) . ?
C40 C42 1.531(4) . ?
C40 C43 1.537(5) . ?
C6 C11 1.400(4) . ?
C11 C10 1.402(4) . ?
C11 C15 1.515(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.384(4) . ?
C21 C20 1.372(4) . ?
C1 C4 1.517(4) . ?
C12 H12 1.0000 . ?
C12 C13 1.516(5) . ?
C12 C14 1.532(5) . ?
C19 C24 1.528(4) . ?
C19 C20 1.396(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C22 H22 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C8 H8 0.9500 . ?
C8 C9 1.374(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.376(5) . ?
C10 H10 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C30 C31 1.533(4) . ?
C30 C32 1.558(5) . ?
C30 C33 1.499(5) . ?
C24 H24 1.0000 . ?
C24 C25 1.542(5) . ?
C24 C26 1.533(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C17 1.515(6) . ?
C15 C16 1.498(6) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C20 H20 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Nb1 N1 83.23(8) . . ?
N3 Nb1 N2 103.09(10) . . ?
N3 Nb1 N4 100.86(11) . . ?
N3 Nb1 N1 99.32(10) . . ?
N3 Nb1 C38 108.17(12) . . ?
N4 Nb1 N2 96.57(9) . . ?
N4 Nb1 N1 159.31(9) . . ?
N4 Nb1 C38 88.62(10) . . ?
C38 Nb1 N2 146.72(11) . . ?
C38 Nb1 N1 80.77(10) . . ?
C18 N2 Nb1 122.66(17) . . ?
C3 N2 Nb1 119.57(18) . . ?
C3 N2 C18 116.7(2) . . ?
C30 N3 Nb1 172.0(2) . . ?
Nb1 N4 H4 117(2) . . ?
C34 N4 Nb1 137.38(19) . . ?
C34 N4 H4 104(2) . . ?
C6 N1 Nb1 125.85(17) . . ?
C1 N1 Nb1 119.39(18) . . ?
C1 N1 C6 114.4(2) . . ?
C23 C27 H27 107.8 . . ?
C23 C27 C28 114.2(3) . . ?
C23 C27 C29 110.2(3) . . ?
C28 C27 H27 107.8 . . ?
C28 C27 C29 108.8(3) . . ?
C29 C27 H27 107.8 . . ?
C18 C23 C27 121.9(2) . . ?
C22 C23 C27 119.4(3) . . ?
C22 C23 C18 118.7(3) . . ?
C23 C18 N2 118.3(2) . . ?
C23 C18 C19 120.1(3) . . ?
C19 C18 N2 121.6(2) . . ?
C1 C2 H2 115.6 . . ?
C3 C2 H2 115.6 . . ?
C3 C2 C1 128.8(3) . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
C38 C39 C40 179.1(4) . . ?
C6 C7 C12 122.5(3) . . ?
C8 C7 C6 118.0(3) . . ?
C8 C7 C12 119.5(3) . . ?
N4 C34 C35 108.2(2) . . ?
N4 C34 C36 108.2(2) . . ?
N4 C34 C37 110.3(3) . . ?
C35 C34 C36 110.6(3) . . ?
C37 C34 C35 109.4(3) . . ?
C37 C34 C36 110.2(3) . . ?
C39 C40 C41 109.6(3) . . ?
C39 C40 C42 109.4(3) . . ?
C39 C40 C43 109.1(3) . . ?
C41 C40 C42 110.2(3) . . ?
C41 C40 C43 109.6(3) . . ?
C42 C40 C43 109.0(3) . . ?
C7 C6 N1 120.1(3) . . ?
C11 C6 N1 118.9(3) . . ?
C11 C6 C7 121.0(3) . . ?
C6 C11 C10 118.3(3) . . ?
C6 C11 C15 122.4(3) . . ?
C10 C11 C15 119.3(3) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C20 C21 C22 119.5(3) . . ?
N1 C1 C2 124.3(3) . . ?
N1 C1 C4 122.0(3) . . ?
C2 C1 C4 113.6(3) . . ?
C7 C12 H12 107.5 . . ?
C7 C12 C14 112.1(3) . . ?
C13 C12 C7 111.7(3) . . ?
C13 C12 H12 107.5 . . ?
C13 C12 C14 110.2(3) . . ?
C14 C12 H12 107.5 . . ?
C18 C19 C24 123.7(3) . . ?
C20 C19 C18 118.7(3) . . ?
C20 C19 C24 117.6(3) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C23 C22 H22 119.4 . . ?
C21 C22 C23 121.3(3) . . ?
C21 C22 H22 119.4 . . ?
N2 C3 C2 124.9(3) . . ?
N2 C3 C5 120.2(3) . . ?
C2 C3 C5 115.0(3) . . ?
C39 C38 Nb1 168.3(3) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C7 C8 H8 119.3 . . ?
C9 C8 C7 121.4(3) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.1(3) . . ?
C10 C9 H9 120.0 . . ?
C11 C10 H10 119.6 . . ?
C9 C10 C11 120.9(3) . . ?
C9 C10 H10 119.6 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N3 C30 C31 109.7(3) . . ?
N3 C30 C32 106.7(3) . . ?
N3 C30 C33 110.6(3) . . ?
C31 C30 C32 109.0(3) . . ?
C33 C30 C31 110.5(3) . . ?
C33 C30 C32 110.2(3) . . ?
C19 C24 H24 108.3 . . ?
C19 C24 C25 111.6(3) . . ?
C19 C24 C26 112.0(3) . . ?
C25 C24 H24 108.3 . . ?
C26 C24 H24 108.3 . . ?
C26 C24 C25 108.5(3) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C11 C15 H15 107.2 . . ?
C17 C15 C11 111.8(3) . . ?
C17 C15 H15 107.2 . . ?
C16 C15 C11 112.0(3) . . ?
C16 C15 H15 107.2 . . ?
C16 C15 C17 111.2(4) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C21 C20 C19 121.7(3) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nb1 N2 C18 C23 100.6(3) . . . . ?
Nb1 N2 C18 C19 -81.0(3) . . . . ?
Nb1 N2 C3 C2 -25.5(4) . . . . ?
Nb1 N2 C3 C5 154.8(2) . . . . ?
Nb1 N4 C34 C35 15.5(4) . . . . ?
Nb1 N4 C34 C36 -104.3(3) . . . . ?
Nb1 N4 C34 C37 135.1(3) . . . . ?
Nb1 N1 C6 C7 83.6(3) . . . . ?
Nb1 N1 C6 C11 -98.7(3) . . . . ?
Nb1 N1 C1 C2 16.3(4) . . . . ?
Nb1 N1 C1 C4 -167.6(2) . . . . ?
N2 C18 C19 C24 -0.1(5) . . . . ?
N2 C18 C19 C20 -178.7(3) . . . . ?
N1 C6 C11 C10 -171.6(3) . . . . ?
N1 C6 C11 C15 8.2(5) . . . . ?
C27 C23 C18 N2 2.8(4) . . . . ?
C27 C23 C18 C19 -175.6(3) . . . . ?
C27 C23 C22 C21 175.5(3) . . . . ?
C23 C18 C19 C24 178.3(3) . . . . ?
C23 C18 C19 C20 -0.4(4) . . . . ?
C18 N2 C3 C2 166.0(3) . . . . ?
C18 N2 C3 C5 -13.7(4) . . . . ?
C18 C23 C22 C21 -1.6(4) . . . . ?
C18 C19 C24 C25 -116.2(3) . . . . ?
C18 C19 C24 C26 122.0(3) . . . . ?
C18 C19 C20 C21 -0.5(5) . . . . ?
C7 C6 C11 C10 6.0(5) . . . . ?
C7 C6 C11 C15 -174.2(3) . . . . ?
C7 C8 C9 C10 2.6(5) . . . . ?
C6 N1 C1 C2 -170.5(3) . . . . ?
C6 N1 C1 C4 5.6(4) . . . . ?
C6 C7 C12 C13 -130.5(3) . . . . ?
C6 C7 C12 C14 105.3(3) . . . . ?
C6 C7 C8 C9 2.2(4) . . . . ?
C6 C11 C10 C9 -1.0(5) . . . . ?
C6 C11 C15 C17 -108.1(4) . . . . ?
C6 C11 C15 C16 126.4(4) . . . . ?
C1 N1 C6 C7 -89.1(3) . . . . ?
C1 N1 C6 C11 88.6(3) . . . . ?
C1 C2 C3 N2 -16.1(5) . . . . ?
C1 C2 C3 C5 163.6(3) . . . . ?
C12 C7 C6 N1 -8.8(4) . . . . ?
C12 C7 C6 C11 173.6(3) . . . . ?
C12 C7 C8 C9 -177.9(3) . . . . ?
C22 C23 C18 N2 179.8(2) . . . . ?
C22 C23 C18 C19 1.3(4) . . . . ?
C22 C21 C20 C19 0.3(5) . . . . ?
C3 N2 C18 C23 -91.3(3) . . . . ?
C3 N2 C18 C19 87.1(3) . . . . ?
C3 C2 C1 N1 20.6(5) . . . . ?
C3 C2 C1 C4 -155.8(3) . . . . ?
C8 C7 C6 N1 171.0(3) . . . . ?
C8 C7 C6 C11 -6.6(4) . . . . ?
C8 C7 C12 C13 49.7(4) . . . . ?
C8 C7 C12 C14 -74.5(4) . . . . ?
C8 C9 C10 C11 -3.2(5) . . . . ?
C10 C11 C15 C17 71.7(4) . . . . ?
C10 C11 C15 C16 -53.8(5) . . . . ?
C28 C27 C23 C18 -146.8(3) . . . . ?
C28 C27 C23 C22 36.3(4) . . . . ?
C24 C19 C20 C21 -179.2(3) . . . . ?
C29 C27 C23 C18 90.4(3) . . . . ?
C29 C27 C23 C22 -86.5(3) . . . . ?
C15 C11 C10 C9 179.1(3) . . . . ?
C20 C21 C22 C23 0.7(5) . . . . ?
C20 C19 C24 C25 62.4(4) . . . . ?
C20 C19 C24 C26 -59.3(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-Hexane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bmkxr31_sq
_database_code_depnum_ccdc_archive 'CCDC 2004175'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-15 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT213_bmkxr31_sq          
;
PROBLEM: Atom C77             has ADP max/min Ratio .....        4.1 prolat
RESPONSE: Possible minor unresolved disorder. 
;
# end Validation Reply Form
_audit_creation_date             2020-05-13
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            '[(BDI)Nb(NtBu)(μ-O2CN(tBu)CO2)]2'
_chemical_name_systematic        
'bis(μ2-(tert-butyl)iminodicarboxylato)-bis(tert-butyl)imino-bis(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-diniobium(V) toluene solvate'
_chemical_formula_moiety         'C78 H118 N8 Nb2 O8, C7 H8'
_chemical_formula_sum            'C85 H126 N8 Nb2 O8'
_chemical_formula_weight         1573.75
_chemical_melting_point          451
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.1406(16)
_cell_length_b                   25.100(3)
_cell_length_c                   22.772(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.348(5)
_cell_angle_gamma                90
_cell_volume                     9125.1(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.46
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6712
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0702 before and 0.0511 after correction.
The Ratio of minimum to maximum transmission is 0.9007.
The λ/2 correction factor is 0.0000.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3352
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.0966
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            71870
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.415
_diffrn_reflns_theta_min         1.257
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11211
_reflns_number_total             16734
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         16734
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0494
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0468P)²+2.3240P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1179
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C51(H51), C54(H54), C63(H63), C66(H66)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C41(H41),
 C47(H47), C48(H48), C49(H49), C59(H59), C60(H60), C61(H61), C81(H81), C82(H82),
  C83(H83), C84(H84), C85(H85)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C64(H64A,
 H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C),
 C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C76(H76A,H76B,
 H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1409(2) 0.31393(14) 0.10459(18) 0.0157(8) Uani 1 1 d . . . . .
C2 C -0.1547(2) 0.27856(14) 0.14777(18) 0.0151(9) Uani 1 1 d . . . . .
H2 H -0.184240 0.293039 0.172169 0.018 Uiso 1 1 calc R . . . .
C3 C -0.1311(2) 0.22523(14) 0.15991(18) 0.0135(8) Uani 1 1 d . . . . .
C4 C -0.2048(2) 0.35838(16) 0.0825(2) 0.0265(10) Uani 1 1 d . . . . .
H4A H -0.199406 0.382027 0.118047 0.040 Uiso 1 1 calc GR . . . .
H4B H -0.261258 0.343133 0.066162 0.040 Uiso 1 1 calc GR . . . .
H4C H -0.194924 0.378724 0.049164 0.040 Uiso 1 1 calc GR . . . .
C5 C -0.1789(2) 0.19429(14) 0.19321(19) 0.0185(9) Uani 1 1 d . . . . .
H5A H -0.167563 0.156143 0.191721 0.028 Uiso 1 1 calc GR . . . .
H5B H -0.239040 0.200845 0.172187 0.028 Uiso 1 1 calc GR . . . .
H5C H -0.160873 0.205896 0.237249 0.028 Uiso 1 1 calc GR . . . .
C6 C -0.0758(2) 0.34522(14) 0.03425(18) 0.0141(8) Uani 1 1 d . . . . .
C7 C -0.0506(2) 0.39839(15) 0.05086(19) 0.0189(9) Uani 1 1 d . . . . .
C8 C -0.0520(2) 0.43249(16) 0.0026(2) 0.0240(10) Uani 1 1 d . . . . .
H8 H -0.037043 0.468760 0.012403 0.029 Uiso 1 1 calc R . . . .
C9 C -0.0740(2) 0.41598(16) -0.0589(2) 0.0258(10) Uani 1 1 d . . . . .
H9 H -0.072667 0.440180 -0.090561 0.031 Uiso 1 1 calc R . . . .
C10 C -0.0979(2) 0.36379(15) -0.07380(19) 0.0211(9) Uani 1 1 d . . . . .
H10 H -0.112930 0.352115 -0.116171 0.025 Uiso 1 1 calc R . . . .
C11 C -0.1007(2) 0.32785(15) -0.02804(18) 0.0163(9) Uani 1 1 d . . . . .
C12 C -0.0235(2) 0.42073(15) 0.1171(2) 0.0253(10) Uani 1 1 d . . . . .
H12 H -0.030889 0.392329 0.145438 0.030 Uiso 1 1 calc R . . . .
C13 C -0.0754(3) 0.46972(17) 0.1216(2) 0.0387(13) Uani 1 1 d . . . . .
H13A H -0.063999 0.499375 0.097923 0.058 Uiso 1 1 calc GR . . . .
H13B H -0.059992 0.480026 0.165924 0.058 Uiso 1 1 calc GR . . . .
H13C H -0.135152 0.460867 0.103900 0.058 Uiso 1 1 calc GR . . . .
C14 C 0.0699(2) 0.43615(15) 0.1407(2) 0.0266(10) Uani 1 1 d . . . . .
H14A H 0.103750 0.404265 0.142558 0.040 Uiso 1 1 calc GR . . . .
H14B H 0.086291 0.451932 0.182813 0.040 Uiso 1 1 calc GR . . . .
H14C H 0.079112 0.462047 0.111642 0.040 Uiso 1 1 calc GR . . . .
C15 C -0.1378(2) 0.27301(15) -0.04832(19) 0.0192(9) Uani 1 1 d . . . . .
H15 H -0.113380 0.248310 -0.011719 0.023 Uiso 1 1 calc R . . . .
C16 C -0.2329(2) 0.27560(17) -0.0642(2) 0.0305(11) Uani 1 1 d . . . . .
H16A H -0.244005 0.286559 -0.026645 0.046 Uiso 1 1 calc GR . . . .
H16B H -0.257503 0.240392 -0.077880 0.046 Uiso 1 1 calc GR . . . .
H16C H -0.257790 0.301486 -0.098058 0.046 Uiso 1 1 calc GR . . . .
C17 C -0.1188(2) 0.25030(17) -0.1036(2) 0.0298(10) Uani 1 1 d . . . . .
H17A H -0.147598 0.271537 -0.141448 0.045 Uiso 1 1 calc GR . . . .
H17B H -0.138398 0.213338 -0.110962 0.045 Uiso 1 1 calc GR . . . .
H17C H -0.058290 0.251392 -0.094050 0.045 Uiso 1 1 calc GR . . . .
C18 C -0.0724(2) 0.14474(14) 0.13938(18) 0.0129(8) Uani 1 1 d . . . . .
C19 C -0.1292(2) 0.12022(14) 0.08453(17) 0.0127(8) Uani 1 1 d . . . . .
C20 C -0.1308(2) 0.06455(14) 0.08179(19) 0.0166(9) Uani 1 1 d . . . . .
H20 H -0.170054 0.047288 0.046100 0.020 Uiso 1 1 calc R . . . .
C21 C -0.0768(2) 0.03431(15) 0.12974(19) 0.0197(9) Uani 1 1 d . . . . .
H21 H -0.077519 -0.003410 0.126197 0.024 Uiso 1 1 calc R . . . .
C22 C -0.0216(2) 0.05850(15) 0.18282(18) 0.0181(9) Uani 1 1 d . . . . .
H22 H 0.015242 0.037051 0.215583 0.022 Uiso 1 1 calc R . . . .
C23 C -0.0185(2) 0.11366(14) 0.18971(18) 0.0151(9) Uani 1 1 d . . . . .
C24 C -0.1900(2) 0.15149(15) 0.03054(18) 0.0170(9) Uani 1 1 d . . . . .
H24 H -0.172379 0.189697 0.036503 0.020 Uiso 1 1 calc R . . . .
C25 C -0.2793(2) 0.14833(16) 0.0306(2) 0.0249(10) Uani 1 1 d . . . . .
H25A H -0.298023 0.111135 0.025579 0.037 Uiso 1 1 calc GR . . . .
H25B H -0.316972 0.169564 -0.004400 0.037 Uiso 1 1 calc GR . . . .
H25C H -0.280131 0.162260 0.070554 0.037 Uiso 1 1 calc GR . . . .
C26 C -0.1892(2) 0.13367(16) -0.03331(19) 0.0253(10) Uani 1 1 d . . . . .
H26A H -0.133593 0.140092 -0.034878 0.038 Uiso 1 1 calc GR . . . .
H26B H -0.231160 0.153911 -0.066917 0.038 Uiso 1 1 calc GR . . . .
H26C H -0.202286 0.095583 -0.039118 0.038 Uiso 1 1 calc GR . . . .
C27 C 0.0379(2) 0.13752(15) 0.25165(18) 0.0164(9) Uani 1 1 d . . . . .
H27 H 0.040641 0.176878 0.245879 0.020 Uiso 1 1 calc R . . . .
C28 C 0.0018(2) 0.12754(16) 0.30317(19) 0.0233(10) Uani 1 1 d . . . . .
H28A H -0.053917 0.143791 0.290746 0.035 Uiso 1 1 calc GR . . . .
H28B H 0.038788 0.143364 0.342882 0.035 Uiso 1 1 calc GR . . . .
H28C H -0.002705 0.089103 0.308806 0.035 Uiso 1 1 calc GR . . . .
C29 C 0.1278(2) 0.11528(15) 0.27432(19) 0.0224(10) Uani 1 1 d . . . . .
H29A H 0.127119 0.077405 0.284565 0.034 Uiso 1 1 calc GR . . . .
H29B H 0.162973 0.134776 0.311939 0.034 Uiso 1 1 calc GR . . . .
H29C H 0.150625 0.119512 0.240875 0.034 Uiso 1 1 calc GR . . . .
C30 C 0.0851(2) 0.29692(15) 0.27293(19) 0.0195(9) Uani 1 1 d . . . . .
C31 C 0.0211(2) 0.28159(15) 0.30264(19) 0.0229(10) Uani 1 1 d . . . . .
H31A H -0.032570 0.298958 0.279503 0.034 Uiso 1 1 calc GR . . . .
H31B H 0.041412 0.293156 0.346761 0.034 Uiso 1 1 calc GR . . . .
H31C H 0.013444 0.242845 0.300639 0.034 Uiso 1 1 calc GR . . . .
C32 C 0.0980(3) 0.35763(15) 0.2762(2) 0.0301(11) Uani 1 1 d . . . . .
H32A H 0.134955 0.367458 0.253672 0.045 Uiso 1 1 calc GR . . . .
H32B H 0.123579 0.368707 0.320364 0.045 Uiso 1 1 calc GR . . . .
H32C H 0.043805 0.375415 0.256597 0.045 Uiso 1 1 calc GR . . . .
C33 C 0.1686(2) 0.26881(17) 0.3052(2) 0.0283(10) Uani 1 1 d . . . . .
H33A H 0.160729 0.230236 0.299300 0.042 Uiso 1 1 calc GR . . . .
H33B H 0.189941 0.277116 0.350307 0.042 Uiso 1 1 calc GR . . . .
H33C H 0.208867 0.280995 0.286613 0.042 Uiso 1 1 calc GR . . . .
C34 C 0.0856(2) 0.17181(14) 0.09346(18) 0.0122(8) Uani 1 1 d . . . . .
C35 C 0.2146(2) 0.12269(14) 0.12508(19) 0.0145(8) Uani 1 1 d . . . . .
C36 C 0.1018(2) 0.10396(15) 0.01746(19) 0.0179(9) Uani 1 1 d . . . . .
C37 C 0.0241(2) 0.07288(16) 0.0147(2) 0.0277(10) Uani 1 1 d . . . . .
H37A H 0.038483 0.048730 0.050949 0.042 Uiso 1 1 calc GR . . . .
H37B H 0.003186 0.052147 -0.024390 0.042 Uiso 1 1 calc GR . . . .
H37C H -0.019376 0.097789 0.015877 0.042 Uiso 1 1 calc GR . . . .
C38 C 0.0842(3) 0.14121(17) -0.0382(2) 0.0346(11) Uani 1 1 d . . . . .
H38A H 0.039463 0.166019 -0.039597 0.052 Uiso 1 1 calc GR . . . .
H38B H 0.066805 0.120400 -0.077304 0.052 Uiso 1 1 calc GR . . . .
H38C H 0.135100 0.161291 -0.033792 0.052 Uiso 1 1 calc GR . . . .
C39 C 0.1685(2) 0.06444(17) 0.0174(2) 0.0403(13) Uani 1 1 d . . . . .
H39A H 0.219631 0.083657 0.020492 0.060 Uiso 1 1 calc GR . . . .
H39B H 0.148501 0.043775 -0.021793 0.060 Uiso 1 1 calc GR . . . .
H39C H 0.180600 0.040310 0.053468 0.060 Uiso 1 1 calc GR . . . .
C40 C 0.5321(2) 0.11990(14) 0.14747(18) 0.0147(8) Uani 1 1 d . . . . .
C41 C 0.5825(2) 0.15589(15) 0.19310(18) 0.0167(9) Uani 1 1 d . . . . .
H41 H 0.633321 0.141784 0.222098 0.020 Uiso 1 1 calc R . . . .
C42 C 0.5675(2) 0.20927(15) 0.20126(18) 0.0157(9) Uani 1 1 d . . . . .
C43 C 0.5801(2) 0.07802(15) 0.12584(19) 0.0210(9) Uani 1 1 d . . . . .
H43A H 0.543813 0.047216 0.108762 0.031 Uiso 1 1 calc GR . . . .
H43B H 0.629450 0.066733 0.161750 0.031 Uiso 1 1 calc GR . . . .
H43C H 0.597986 0.093174 0.093105 0.031 Uiso 1 1 calc GR . . . .
C44 C 0.6414(2) 0.24085(15) 0.24339(19) 0.0232(10) Uani 1 1 d . . . . .
H44A H 0.642041 0.275846 0.224500 0.035 Uiso 1 1 calc GR . . . .
H44B H 0.693270 0.221765 0.248303 0.035 Uiso 1 1 calc GR . . . .
H44C H 0.636947 0.245482 0.284795 0.035 Uiso 1 1 calc GR . . . .
C45 C 0.40754(19) 0.08443(14) 0.07301(17) 0.0115(8) Uani 1 1 d . . . . .
C46 C 0.3860(2) 0.03487(14) 0.09194(19) 0.0165(9) Uani 1 1 d . . . . .
C47 C 0.3549(2) -0.00383(15) 0.0454(2) 0.0229(10) Uani 1 1 d . . . . .
H47 H 0.342088 -0.038111 0.057166 0.027 Uiso 1 1 calc R . . . .
C48 C 0.3419(2) 0.00584(16) -0.0172(2) 0.0251(10) Uani 1 1 d . . . . .
H48 H 0.320415 -0.021415 -0.047840 0.030 Uiso 1 1 calc R . . . .
C49 C 0.3602(2) 0.05466(15) -0.03470(19) 0.0207(9) Uani 1 1 d . . . . .
H49 H 0.350553 0.061361 -0.077847 0.025 Uiso 1 1 calc R . . . .
C50 C 0.3931(2) 0.09535(14) 0.00973(18) 0.0155(9) Uani 1 1 d . . . . .
C51 C 0.3964(2) 0.02331(15) 0.1595(2) 0.0253(10) Uani 1 1 d . . . . .
H51 H 0.388306 0.057722 0.178732 0.030 Uiso 1 1 calc R . . . .
C52 C 0.3319(2) -0.01613(16) 0.1662(2) 0.0332(11) Uani 1 1 d . . . . .
H52A H 0.275637 -0.005531 0.138122 0.050 Uiso 1 1 calc GR . . . .
H52B H 0.334446 -0.016117 0.209939 0.050 Uiso 1 1 calc GR . . . .
H52C H 0.344278 -0.051961 0.154925 0.050 Uiso 1 1 calc GR . . . .
C53 C 0.4842(2) 0.00278(17) 0.1991(2) 0.0363(12) Uani 1 1 d . . . . .
H53A H 0.499552 -0.026116 0.176492 0.055 Uiso 1 1 calc GR . . . .
H53B H 0.484340 -0.010541 0.239631 0.055 Uiso 1 1 calc GR . . . .
H53C H 0.524736 0.031905 0.206567 0.055 Uiso 1 1 calc GR . . . .
C54 C 0.4138(2) 0.14846(16) -0.01217(19) 0.0221(9) Uani 1 1 d . . . . .
H54 H 0.436178 0.172126 0.025616 0.026 Uiso 1 1 calc R . . . .
C55 C 0.3365(2) 0.17529(17) -0.0590(2) 0.0315(11) Uani 1 1 d . . . . .
H55A H 0.312757 0.152703 -0.096394 0.047 Uiso 1 1 calc GR . . . .
H55B H 0.352207 0.209875 -0.071346 0.047 Uiso 1 1 calc GR . . . .
H55C H 0.294844 0.180555 -0.039346 0.047 Uiso 1 1 calc GR . . . .
C56 C 0.4822(2) 0.14277(19) -0.0403(2) 0.0352(12) Uani 1 1 d . . . . .
H56A H 0.531775 0.125932 -0.009390 0.053 Uiso 1 1 calc GR . . . .
H56B H 0.497287 0.178084 -0.051237 0.053 Uiso 1 1 calc GR . . . .
H56C H 0.461371 0.120664 -0.078369 0.053 Uiso 1 1 calc GR . . . .
C57 C 0.4902(2) 0.29002(14) 0.16550(18) 0.0142(8) Uani 1 1 d . . . . .
C58 C 0.4977(2) 0.31163(15) 0.11049(19) 0.0177(9) Uani 1 1 d . . . . .
C59 C 0.4914(2) 0.36675(16) 0.1020(2) 0.0302(11) Uani 1 1 d . . . . .
H59 H 0.495911 0.381867 0.065142 0.036 Uiso 1 1 calc R . . . .
C60 C 0.4788(3) 0.39960(17) 0.1461(3) 0.0443(13) Uani 1 1 d . . . . .
H60 H 0.474093 0.437001 0.139358 0.053 Uiso 1 1 calc R . . . .
C61 C 0.4730(3) 0.37846(17) 0.1995(2) 0.0337(11) Uani 1 1 d . . . . .
H61 H 0.464358 0.401674 0.229533 0.040 Uiso 1 1 calc R . . . .
C62 C 0.4794(2) 0.32380(16) 0.2115(2) 0.0229(10) Uani 1 1 d . . . . .
C63 C 0.5136(2) 0.27699(15) 0.06169(19) 0.0184(9) Uani 1 1 d . . . . .
H63 H 0.483542 0.242526 0.059849 0.022 Uiso 1 1 calc R . . . .
C64 C 0.4820(3) 0.3003(2) -0.0041(2) 0.0434(13) Uani 1 1 d . . . . .
H64A H 0.423002 0.310362 -0.015898 0.065 Uiso 1 1 calc GR . . . .
H64B H 0.487478 0.273830 -0.033926 0.065 Uiso 1 1 calc GR . . . .
H64C H 0.515076 0.331972 -0.004979 0.065 Uiso 1 1 calc GR . . . .
C65 C 0.6054(3) 0.2643(2) 0.0794(3) 0.0593(17) Uani 1 1 d . . . . .
H65A H 0.637149 0.297530 0.084053 0.089 Uiso 1 1 calc GR . . . .
H65B H 0.613188 0.242491 0.046243 0.089 Uiso 1 1 calc GR . . . .
H65C H 0.625476 0.244687 0.119314 0.089 Uiso 1 1 calc GR . . . .
C66 C 0.4776(2) 0.30417(16) 0.27408(19) 0.0218(9) Uani 1 1 d . . . . .
H66 H 0.479310 0.264350 0.274124 0.026 Uiso 1 1 calc R . . . .
C67 C 0.3984(2) 0.32170(17) 0.2846(2) 0.0289(11) Uani 1 1 d . . . . .
H67A H 0.397253 0.360651 0.287084 0.043 Uiso 1 1 calc GR . . . .
H67B H 0.398020 0.306327 0.324078 0.043 Uiso 1 1 calc GR . . . .
H67C H 0.348992 0.309350 0.249437 0.043 Uiso 1 1 calc GR . . . .
C68 C 0.5541(2) 0.32442(18) 0.3291(2) 0.0315(11) Uani 1 1 d . . . . .
H68A H 0.604833 0.318430 0.319675 0.047 Uiso 1 1 calc GR . . . .
H68B H 0.558600 0.305158 0.367622 0.047 Uiso 1 1 calc GR . . . .
H68C H 0.547757 0.362605 0.335129 0.047 Uiso 1 1 calc GR . . . .
C69 C 0.4206(2) 0.14646(16) 0.29757(18) 0.0225(9) Uani 1 1 d . . . . .
C70 C 0.3553(2) 0.1775(2) 0.3155(2) 0.0404(12) Uani 1 1 d . . . . .
H70A H 0.364322 0.215805 0.312736 0.061 Uiso 1 1 calc GR . . . .
H70B H 0.360960 0.168367 0.358710 0.061 Uiso 1 1 calc GR . . . .
H70C H 0.298960 0.168059 0.286500 0.061 Uiso 1 1 calc GR . . . .
C71 C 0.5098(2) 0.16178(17) 0.34115(19) 0.0299(11) Uani 1 1 d . . . . .
H71A H 0.550555 0.143972 0.326861 0.045 Uiso 1 1 calc GR . . . .
H71B H 0.518758 0.150669 0.384385 0.045 Uiso 1 1 calc GR . . . .
H71C H 0.516775 0.200464 0.339977 0.045 Uiso 1 1 calc GR . . . .
C72 C 0.4082(3) 0.08685(17) 0.3008(2) 0.0416(13) Uani 1 1 d . . . . .
H72A H 0.353091 0.076896 0.270211 0.062 Uiso 1 1 calc GR . . . .
H72B H 0.411599 0.077161 0.343306 0.062 Uiso 1 1 calc GR . . . .
H72C H 0.451921 0.067990 0.290814 0.062 Uiso 1 1 calc GR . . . .
C73 C 0.2873(2) 0.26394(14) 0.10361(18) 0.0122(8) Uani 1 1 d . . . . .
C74 C 0.1765(2) 0.31152(14) 0.12074(18) 0.0127(8) Uani 1 1 d . . . . .
C75 C 0.1971(2) 0.32278(15) 0.01518(18) 0.0184(9) Uani 1 1 d . . . . .
C76 C 0.1439(2) 0.37218(15) 0.0125(2) 0.0243(10) Uani 1 1 d . . . . .
H76A H 0.093498 0.361939 0.020546 0.036 Uiso 1 1 calc GR . . . .
H76B H 0.127629 0.388547 -0.029314 0.036 Uiso 1 1 calc GR . . . .
H76C H 0.176391 0.397770 0.044602 0.036 Uiso 1 1 calc GR . . . .
C77 C 0.2720(2) 0.33903(19) -0.0007(2) 0.0416(13) Uani 1 1 d . . . . .
H77A H 0.306620 0.364097 0.031124 0.062 Uiso 1 1 calc GR . . . .
H77B H 0.252855 0.356126 -0.042266 0.062 Uiso 1 1 calc GR . . . .
H77C H 0.305227 0.307389 -0.001365 0.062 Uiso 1 1 calc GR . . . .
C78 C 0.1457(3) 0.28084(17) -0.0304(2) 0.0342(11) Uani 1 1 d . . . . .
H78A H 0.180656 0.249458 -0.028359 0.051 Uiso 1 1 calc GR . . . .
H78B H 0.125540 0.295277 -0.073379 0.051 Uiso 1 1 calc GR . . . .
H78C H 0.097828 0.270675 -0.019118 0.051 Uiso 1 1 calc GR . . . .
C79 C 0.2983(3) 0.5398(3) 0.1454(3) 0.087(2) Uani 1 1 d . . . . .
H79A H 0.252400 0.559623 0.114343 0.130 Uiso 1 1 calc GR . . . .
H79B H 0.312374 0.508802 0.125026 0.130 Uiso 1 1 calc GR . . . .
H79C H 0.347425 0.562937 0.162458 0.130 Uiso 1 1 calc GR . . . .
C80 C 0.2713(3) 0.5213(2) 0.1984(2) 0.0457(14) Uani 1 1 d . . . . .
C81 C 0.2885(3) 0.4698(2) 0.2220(3) 0.0469(14) Uani 1 1 d . . . . .
H81 H 0.316218 0.445779 0.203898 0.056 Uiso 1 1 calc R . . . .
C82 C 0.2664(2) 0.45340(19) 0.2701(3) 0.0408(13) Uani 1 1 d . . . . .
H82 H 0.279714 0.418237 0.286056 0.049 Uiso 1 1 calc R . . . .
C83 C 0.2243(2) 0.48763(17) 0.2968(2) 0.0299(11) Uani 1 1 d . . . . .
H83 H 0.209055 0.475903 0.330827 0.036 Uiso 1 1 calc R . . . .
C84 C 0.2049(2) 0.53825(16) 0.2735(2) 0.0279(11) Uani 1 1 d . . . . .
H84 H 0.175809 0.561778 0.291017 0.034 Uiso 1 1 calc R . . . .
C85 C 0.2283(2) 0.55485(19) 0.2242(2) 0.0374(12) Uani 1 1 d . . . . .
H85 H 0.214462 0.589850 0.207831 0.045 Uiso 1 1 calc R . . . .
N1 N -0.07867(16) 0.30812(11) 0.08301(14) 0.0125(7) Uani 1 1 d . . . . .
N2 N -0.07179(16) 0.20228(11) 0.14317(14) 0.0114(7) Uani 1 1 d . . . . .
N3 N 0.05335(16) 0.28062(11) 0.20695(14) 0.0112(7) Uani 1 1 d . . . . .
N4 N 0.13148(16) 0.13447(12) 0.07851(15) 0.0148(7) Uani 1 1 d . . . . .
N5 N 0.44932(16) 0.12391(11) 0.12106(14) 0.0101(7) Uani 1 1 d . . . . .
N6 N 0.49262(16) 0.23259(11) 0.17303(14) 0.0112(7) Uani 1 1 d . . . . .
N7 N 0.40908(16) 0.16054(11) 0.23315(14) 0.0134(7) Uani 1 1 d . . . . .
N8 N 0.22675(16) 0.30123(11) 0.08145(14) 0.0128(7) Uani 1 1 d . . . . .
O1 O 0.11395(13) 0.19186(9) 0.15050(12) 0.0133(6) Uani 1 1 d . . . . .
O2 O 0.01683(13) 0.19011(9) 0.05502(12) 0.0139(6) Uani 1 1 d . . . . .
O3 O 0.27349(13) 0.14400(9) 0.10894(12) 0.0142(6) Uani 1 1 d . . . . .
O4 O 0.22324(15) 0.09478(11) 0.16980(14) 0.0249(7) Uani 1 1 d . . . . .
O5 O 0.30709(13) 0.24767(9) 0.16161(11) 0.0126(5) Uani 1 1 d . . . . .
O6 O 0.32480(13) 0.24250(9) 0.07073(11) 0.0139(6) Uani 1 1 d . . . . .
O7 O 0.10072(13) 0.29280(9) 0.09442(11) 0.0129(6) Uani 1 1 d . . . . .
O8 O 0.20627(14) 0.33491(10) 0.16967(13) 0.0195(6) Uani 1 1 d . . . . .
Nb1 Nb 0.02448(2) 0.25335(2) 0.13138(2) 0.01036(9) Uani 1 1 d . . . . .
Nb2 Nb 0.38197(2) 0.18398(2) 0.15565(2) 0.01058(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.407(5) . ?
C1 C4 1.515(5) . ?
C1 N1 1.335(4) . ?
C2 C3 1.397(5) . ?
C3 C5 1.517(5) . ?
C3 N2 1.339(4) . ?
C6 C7 1.411(5) . ?
C6 C11 1.394(5) . ?
C6 N1 1.464(5) . ?
C7 C8 1.387(5) . ?
C7 C12 1.515(5) . ?
C8 C9 1.374(6) . ?
C9 C10 1.378(5) . ?
C10 C11 1.392(5) . ?
C11 C15 1.516(5) . ?
C12 C13 1.543(5) . ?
C12 C14 1.542(5) . ?
C15 C16 1.538(5) . ?
C15 C17 1.521(5) . ?
C18 C19 1.415(5) . ?
C18 C23 1.416(5) . ?
C18 N2 1.447(4) . ?
C19 C20 1.398(5) . ?
C19 C24 1.510(5) . ?
C20 C21 1.375(5) . ?
C21 C22 1.375(5) . ?
C22 C23 1.392(5) . ?
C23 C27 1.513(5) . ?
C24 C25 1.533(5) . ?
C24 C26 1.526(5) . ?
C27 C28 1.534(5) . ?
C27 C29 1.541(5) . ?
C30 C31 1.533(5) . ?
C30 C32 1.538(5) . ?
C30 C33 1.523(5) . ?
C30 N3 1.458(5) . ?
C34 N4 1.345(4) . ?
C34 O1 1.310(4) . ?
C34 O2 1.271(4) . ?
C34 Nb1 2.586(4) . ?
C35 N4 1.463(4) . ?
C35 O3 1.308(4) . ?
C35 O4 1.200(4) . ?
C36 C37 1.525(5) . ?
C36 C38 1.515(6) . ?
C36 C39 1.515(5) . ?
C36 N4 1.504(5) . ?
C40 C41 1.410(5) . ?
C40 C43 1.523(5) . ?
C40 N5 1.329(4) . ?
C41 C42 1.389(5) . ?
C42 C44 1.506(5) . ?
C42 N6 1.342(4) . ?
C45 C46 1.409(5) . ?
C45 C50 1.398(5) . ?
C45 N5 1.456(4) . ?
C46 C47 1.392(5) . ?
C46 C51 1.512(6) . ?
C47 C48 1.384(6) . ?
C48 C49 1.360(5) . ?
C49 C50 1.403(5) . ?
C50 C54 1.510(5) . ?
C51 C52 1.532(5) . ?
C51 C53 1.535(5) . ?
C54 C55 1.522(5) . ?
C54 C56 1.535(5) . ?
C57 C58 1.413(5) . ?
C57 C62 1.411(5) . ?
C57 N6 1.450(4) . ?
C58 C59 1.396(5) . ?
C58 C63 1.512(5) . ?
C59 C60 1.376(6) . ?
C60 C61 1.363(6) . ?
C61 C62 1.395(5) . ?
C62 C66 1.519(6) . ?
C63 C64 1.513(6) . ?
C63 C65 1.509(5) . ?
C66 C67 1.528(5) . ?
C66 C68 1.533(5) . ?
C69 C70 1.536(6) . ?
C69 C71 1.537(5) . ?
C69 C72 1.517(6) . ?
C69 N7 1.451(5) . ?
C73 N8 1.352(4) . ?
C73 O5 1.304(4) . ?
C73 O6 1.270(4) . ?
C73 Nb2 2.581(4) . ?
C74 N8 1.473(5) . ?
C74 O7 1.303(4) . ?
C74 O8 1.197(4) . ?
C75 C76 1.527(5) . ?
C75 C77 1.513(5) . ?
C75 C78 1.515(5) . ?
C75 N8 1.507(5) . ?
C79 C80 1.515(7) . ?
C80 C81 1.389(7) . ?
C80 C85 1.383(7) . ?
C81 C82 1.347(7) . ?
C82 C83 1.396(6) . ?
C83 C84 1.370(5) . ?
C84 C85 1.386(6) . ?
N1 Nb1 2.193(3) . ?
N2 Nb1 2.182(3) . ?
N3 Nb1 1.748(3) . ?
N5 Nb2 2.211(3) . ?
N6 Nb2 2.167(3) . ?
N7 Nb2 1.755(3) . ?
O1 Nb1 2.106(2) . ?
O2 Nb1 2.323(2) . ?
O3 Nb2 2.039(2) . ?
O5 Nb2 2.085(2) . ?
O6 Nb2 2.340(2) . ?
O7 Nb1 2.049(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C4 114.3(3) . . ?
N1 C1 C2 123.2(3) . . ?
N1 C1 C4 122.4(3) . . ?
C3 C2 C1 129.3(3) . . ?
C2 C3 C5 114.8(3) . . ?
N2 C3 C2 123.4(3) . . ?
N2 C3 C5 121.7(3) . . ?
C7 C6 N1 119.3(3) . . ?
C11 C6 C7 121.3(4) . . ?
C11 C6 N1 119.4(3) . . ?
C6 C7 C12 124.8(4) . . ?
C8 C7 C6 117.1(4) . . ?
C8 C7 C12 118.1(3) . . ?
C9 C8 C7 122.7(4) . . ?
C8 C9 C10 119.0(4) . . ?
C9 C10 C11 121.3(4) . . ?
C6 C11 C15 122.2(3) . . ?
C10 C11 C6 118.5(4) . . ?
C10 C11 C15 119.0(4) . . ?
C7 C12 C13 112.7(3) . . ?
C7 C12 C14 110.1(3) . . ?
C14 C12 C13 109.1(3) . . ?
C11 C15 C16 108.9(3) . . ?
C11 C15 C17 113.6(3) . . ?
C17 C15 C16 110.4(3) . . ?
C19 C18 C23 120.8(3) . . ?
C19 C18 N2 118.4(3) . . ?
C23 C18 N2 120.9(3) . . ?
C18 C19 C24 122.8(3) . . ?
C20 C19 C18 118.0(3) . . ?
C20 C19 C24 119.1(3) . . ?
C21 C20 C19 121.3(3) . . ?
C20 C21 C22 120.2(3) . . ?
C21 C22 C23 121.6(4) . . ?
C18 C23 C27 122.9(3) . . ?
C22 C23 C18 118.0(3) . . ?
C22 C23 C27 118.9(3) . . ?
C19 C24 C25 111.5(3) . . ?
C19 C24 C26 112.3(3) . . ?
C26 C24 C25 109.9(3) . . ?
C23 C27 C28 110.4(3) . . ?
C23 C27 C29 113.0(3) . . ?
C28 C27 C29 108.5(3) . . ?
C31 C30 C32 109.9(3) . . ?
C33 C30 C31 111.7(3) . . ?
C33 C30 C32 110.0(3) . . ?
N3 C30 C31 109.0(3) . . ?
N3 C30 C32 108.7(3) . . ?
N3 C30 C33 107.4(3) . . ?
N4 C34 Nb1 168.9(2) . . ?
O1 C34 N4 118.6(3) . . ?
O1 C34 Nb1 54.15(16) . . ?
O2 C34 N4 124.0(3) . . ?
O2 C34 O1 117.4(3) . . ?
O2 C34 Nb1 63.72(18) . . ?
O3 C35 N4 111.2(3) . . ?
O4 C35 N4 121.3(3) . . ?
O4 C35 O3 127.4(3) . . ?
C38 C36 C37 112.2(3) . . ?
C39 C36 C37 108.3(3) . . ?
C39 C36 C38 108.9(4) . . ?
N4 C36 C37 107.2(3) . . ?
N4 C36 C38 110.9(3) . . ?
N4 C36 C39 109.4(3) . . ?
C41 C40 C43 115.0(3) . . ?
N5 C40 C41 123.5(3) . . ?
N5 C40 C43 121.3(3) . . ?
C42 C41 C40 128.6(3) . . ?
C41 C42 C44 116.0(3) . . ?
N6 C42 C41 123.2(3) . . ?
N6 C42 C44 120.8(3) . . ?
C46 C45 N5 118.9(3) . . ?
C50 C45 C46 121.4(3) . . ?
C50 C45 N5 119.7(3) . . ?
C45 C46 C51 122.3(3) . . ?
C47 C46 C45 117.0(4) . . ?
C47 C46 C51 120.7(4) . . ?
C48 C47 C46 122.4(4) . . ?
C49 C48 C47 119.5(4) . . ?
C48 C49 C50 121.3(4) . . ?
C45 C50 C49 118.3(3) . . ?
C45 C50 C54 122.6(3) . . ?
C49 C50 C54 119.0(4) . . ?
C46 C51 C52 113.8(3) . . ?
C46 C51 C53 112.9(3) . . ?
C52 C51 C53 108.3(3) . . ?
C50 C54 C55 111.9(3) . . ?
C50 C54 C56 111.3(3) . . ?
C55 C54 C56 110.6(3) . . ?
C58 C57 N6 118.6(3) . . ?
C62 C57 C58 120.4(3) . . ?
C62 C57 N6 121.0(3) . . ?
C57 C58 C63 122.0(3) . . ?
C59 C58 C57 118.4(4) . . ?
C59 C58 C63 119.6(4) . . ?
C60 C59 C58 121.2(4) . . ?
C61 C60 C59 120.0(4) . . ?
C60 C61 C62 122.1(4) . . ?
C57 C62 C66 123.7(4) . . ?
C61 C62 C57 117.9(4) . . ?
C61 C62 C66 118.4(4) . . ?
C58 C63 C64 114.2(3) . . ?
C65 C63 C58 112.0(3) . . ?
C65 C63 C64 108.0(4) . . ?
C62 C66 C67 112.1(3) . . ?
C62 C66 C68 110.9(3) . . ?
C67 C66 C68 108.7(3) . . ?
C70 C69 C71 110.5(3) . . ?
C72 C69 C70 111.0(4) . . ?
C72 C69 C71 109.9(3) . . ?
N7 C69 C70 107.5(3) . . ?
N7 C69 C71 109.2(3) . . ?
N7 C69 C72 108.6(3) . . ?
N8 C73 Nb2 168.1(2) . . ?
O5 C73 N8 118.4(3) . . ?
O5 C73 Nb2 53.38(16) . . ?
O6 C73 N8 123.9(3) . . ?
O6 C73 O5 117.6(3) . . ?
O6 C73 Nb2 64.72(18) . . ?
O7 C74 N8 111.3(3) . . ?
O8 C74 N8 120.4(3) . . ?
O8 C74 O7 128.4(3) . . ?
C77 C75 C76 108.6(3) . . ?
C77 C75 C78 110.8(4) . . ?
C78 C75 C76 110.3(3) . . ?
N8 C75 C76 108.1(3) . . ?
N8 C75 C77 109.3(3) . . ?
N8 C75 C78 109.7(3) . . ?
C81 C80 C79 120.7(5) . . ?
C85 C80 C79 121.1(5) . . ?
C85 C80 C81 118.2(5) . . ?
C82 C81 C80 121.1(5) . . ?
C81 C82 C83 120.6(5) . . ?
C84 C83 C82 119.5(5) . . ?
C83 C84 C85 119.5(4) . . ?
C80 C85 C84 121.1(5) . . ?
C1 N1 C6 117.5(3) . . ?
C1 N1 Nb1 119.3(2) . . ?
C6 N1 Nb1 122.4(2) . . ?
C3 N2 C18 117.2(3) . . ?
C3 N2 Nb1 118.0(2) . . ?
C18 N2 Nb1 124.6(2) . . ?
C30 N3 Nb1 172.0(3) . . ?
C34 N4 C35 117.5(3) . . ?
C34 N4 C36 123.8(3) . . ?
C35 N4 C36 118.7(3) . . ?
C40 N5 C45 116.1(3) . . ?
C40 N5 Nb2 120.1(2) . . ?
C45 N5 Nb2 123.63(19) . . ?
C42 N6 C57 118.1(3) . . ?
C42 N6 Nb2 117.5(2) . . ?
C57 N6 Nb2 123.5(2) . . ?
C69 N7 Nb2 170.8(3) . . ?
C73 N8 C74 115.7(3) . . ?
C73 N8 C75 123.8(3) . . ?
C74 N8 C75 119.1(3) . . ?
C34 O1 Nb1 95.6(2) . . ?
C34 O2 Nb1 86.9(2) . . ?
C35 O3 Nb2 134.9(2) . . ?
C73 O5 Nb2 96.5(2) . . ?
C73 O6 Nb2 85.9(2) . . ?
C74 O7 Nb1 131.5(2) . . ?
N1 Nb1 C34 132.74(11) . . ?
N1 Nb1 O2 103.70(10) . . ?
N2 Nb1 C34 89.58(10) . . ?
N2 Nb1 N1 85.56(10) . . ?
N2 Nb1 O2 81.46(9) . . ?
N3 Nb1 C34 129.40(12) . . ?
N3 Nb1 N1 97.85(12) . . ?
N3 Nb1 N2 93.71(12) . . ?
N3 Nb1 O1 99.18(11) . . ?
N3 Nb1 O2 157.42(11) . . ?
N3 Nb1 O7 102.75(11) . . ?
O1 Nb1 C34 30.28(10) . . ?
O1 Nb1 N1 162.96(10) . . ?
O1 Nb1 N2 94.04(9) . . ?
O1 Nb1 O2 59.50(9) . . ?
O2 Nb1 C34 29.38(9) . . ?
O7 Nb1 C34 81.31(10) . . ?
O7 Nb1 N1 90.51(10) . . ?
O7 Nb1 N2 163.46(10) . . ?
O7 Nb1 O1 85.05(9) . . ?
O7 Nb1 O2 83.88(9) . . ?
N5 Nb2 C73 133.55(11) . . ?
N5 Nb2 O6 104.45(9) . . ?
N6 Nb2 C73 90.46(10) . . ?
N6 Nb2 N5 85.03(10) . . ?
N6 Nb2 O6 82.70(9) . . ?
N7 Nb2 C73 127.91(13) . . ?
N7 Nb2 N5 98.52(12) . . ?
N7 Nb2 N6 96.39(12) . . ?
N7 Nb2 O3 102.53(11) . . ?
N7 Nb2 O5 97.79(11) . . ?
N7 Nb2 O6 156.82(11) . . ?
O3 Nb2 C73 80.90(10) . . ?
O3 Nb2 N5 88.50(9) . . ?
O3 Nb2 N6 160.72(11) . . ?
O3 Nb2 O5 86.86(9) . . ?
O3 Nb2 O6 81.36(9) . . ?
O5 Nb2 C73 30.12(10) . . ?
O5 Nb2 N5 163.65(10) . . ?
O5 Nb2 N6 94.30(9) . . ?
O5 Nb2 O6 59.34(9) . . ?
O6 Nb2 C73 29.39(10) . . ?

loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
0 3 6 6.265

_platon_squeeze_details          
;
TITL bmkxr31_0m in P2(1)/c
CELL   17.1406   25.1000   22.7720     90.00    111.35     90.00
SPGR P21/c
# Solvent Accessible Volume =      1306
# Electrons Found in S.A.V. =       329
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.189 0.531 0.752 !       6.39 eA-3
C102 0.754 0.382 0.243 !       5.03 eA-3
C103 0.305 0.892 0.297 !       4.78 eA-3
C104 0.258 0.977 0.313 !       4.48 eA-3
C105 0.317 0.563 0.827 !       4.45 eA-3
C106 0.251 0.936 0.290 !       4.29 eA-3
C107 0.821 0.078 0.781 !       4.09 eA-3
C108 0.141 0.891 0.178 !       4.03 eA-3
C109 0.785 0.366 0.273 !       3.89 eA-3
C110 0.530 0.029 0.481 !       3.72 eA-3
C111 0.900 0.411 0.336 !       3.48 eA-3
C112 0.133 0.946 0.184 !       3.46 eA-3
C113 0.596 0.960 0.528 !       2.91 eA-3
C114 0.458 0.494 0.992 !       2.77 eA-3
C115 0.377 0.489 0.000 !       2.01 eA-3
C116 0.328 0.984 0.499 !       1.91 eA-3
C117 0.340 0.026 0.476 !       1.87 eA-3
C118 0.605 0.037 0.480 !       1.83 eA-3
C119 0.721 0.507 0.159 !       1.15 eA-3
C120 0.543 0.581 0.029 !       0.99 eA-3
C121 0.761 0.994 0.671 !       0.97 eA-3
C122 0.640 0.455 0.109 !       0.94 eA-3
Q123 0.663 0.063 0.453 !       0.90 eA-3
C124 0.326 0.932 0.282 !       0.90 eA-3
C125 0.674 0.424 0.121 !       0.89 eA-3
C126 0.920 0.461 0.344 !       0.87 eA-3
C127 0.631 0.037 0.651 !       0.84 eA-3
C128 0.282 0.983 0.461 !       0.83 eA-3
C129 0.871 0.445 0.261 !       0.81 eA-3
C130 0.757 0.473 0.139 !       0.81 eA-3
C131 0.428 0.937 0.475 !       0.80 eA-3
C132 0.564 0.029 0.523 !       0.77 eA-3
Q133 0.706 0.446 0.111 !       0.77 eA-3
C134 0.294 0.643 0.750 !       0.77 eA-3
C135 0.254 0.028 0.454 !       0.76 eA-3
Q136 0.735 0.163 0.693 !       0.75 eA-3
C137 0.401 0.495 0.945 !       0.75 eA-3
C138 0.096 0.572 0.623 !       0.75 eA-3
C139 0.950 0.061 0.828 !       0.75 eA-3
C140 0.835 0.008 0.709 !       0.74 eA-3
C141 0.205 0.637 0.775 !       0.74 eA-3
C142 0.690 0.133 0.659 !       0.73 eA-3
C143 0.062 0.869 0.155 !       0.73 eA-3
C144 0.640 0.087 0.491 !       0.72 eA-3
Q145 0.537 0.571 0.071 !       0.72 eA-3
C146 0.749 0.492 0.048 !       0.71 eA-3
Q147 0.483 0.945 0.459 !       0.70 eA-3
Q148 0.672 0.021 0.463 !       0.70 eA-3
C149 0.165 0.580 0.670 !       0.70 eA-3
C150 0.390 0.568 0.053 !       0.70 eA-3
Q151 0.152 0.733 0.734 !       0.69 eA-3
C152 0.416 0.580 0.046 !       0.69 eA-3
Q153 0.918 0.131 0.726 !       0.69 eA-3
Q154 0.438 0.226 0.492 !       0.69 eA-3
Q155 0.397 0.577 0.884 !       0.69 eA-3
Q156 0.503 0.601 0.083 !       0.68 eA-3
C157 0.475 0.506 0.953 !       0.68 eA-3
Q158 0.624 0.087 0.698 !       0.68 eA-3
Q159 0.568 0.055 0.640 !       0.68 eA-3
Q160 0.717 0.407 0.158 !       0.68 eA-3
C161 0.287 0.069 0.387 !       0.68 eA-3
Q162 0.482 0.111 0.468 !       0.67 eA-3
Q163 0.156 0.086 0.035 !       0.67 eA-3
Q164 0.620 0.956 0.438 !       0.67 eA-3
Q165 0.036 0.554 0.584 !       0.67 eA-3
Q166 0.070 0.460 0.258 !       0.66 eA-3
C167 0.475 0.585 0.037 !       0.65 eA-3
Q168 0.294 0.532 0.773 !       0.65 eA-3
Q169 0.620 0.680 0.345 !       0.65 eA-3
Q170 0.596 0.580 0.002 !       0.65 eA-3
C171 0.661 0.454 0.033 !       0.65 eA-3
Q172 0.026 0.250 0.136 !       0.65 eA-3
Q173 0.382 0.412 0.971 !       0.65 eA-3
Q174 0.753 0.351 0.149 !       0.65 eA-3
C175 0.455 0.530 0.073 !       0.64 eA-3
Q176 0.369 0.546 0.796 !       0.64 eA-3
Q177 0.769 0.635 0.538 !       0.64 eA-3
Q178 0.531 0.030 0.359 !       0.64 eA-3
Q179 0.818 0.041 0.844 !       0.63 eA-3
C180 0.720 0.515 0.074 !       0.63 eA-3
Q181 0.297 0.014 0.313 !       0.63 eA-3
Q182 0.409 0.555 0.115 !       0.63 eA-3
C183 0.211 0.593 0.799 !       0.63 eA-3
Q184 0.036 0.585 0.314 !       0.63 eA-3
Q185 0.737 0.313 0.055 !       0.62 eA-3
Q186 0.145 0.498 0.650 !       0.62 eA-3
Q187 0.555 0.453 0.407 !       0.62 eA-3
C188 0.145 0.970 0.116 !       0.62 eA-3
Q189 0.607 0.219 0.548 !       0.62 eA-3
C190 0.731 0.017 0.593 !       0.62 eA-3
Q191 0.018 0.694 0.329 !       0.62 eA-3
Q192 0.480 0.960 0.426 !       0.61 eA-3
Q193 0.320 0.149 0.139 !       0.61 eA-3
Q194 0.671 0.601 0.128 !       0.61 eA-3
Q195 0.248 0.188 0.219 !       0.61 eA-3
Q196 0.733 0.429 0.117 !       0.61 eA-3
C197 0.384 0.479 0.918 !       0.61 eA-3
Q198 0.302 0.905 0.414 !       0.61 eA-3
C199 0.134 0.834 0.198 !       0.60 eA-3
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 1.000 0.500 653 165 ' '
2 0.500 0.500 1.000 653 165 ' '

_platon_squeeze_void_probe_radius 1.20

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Toluene'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bmkxr49
_database_code_depnum_ccdc_archive 'CCDC 2004312'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-17 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_audit_creation_date             2020-05-16
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            (BDI)NbH(N[BO2C6H12]tBu)(NtBu)
_chemical_name_systematic        
hydrido-(N-(tert-butyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-amino)-(tert-butyl)imino-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V)
_chemical_formula_moiety         'C43 H72 B N4 Nb O2'
_chemical_formula_sum            'C43 H72 B N4 Nb O2'
_chemical_formula_weight         780.76
_chemical_melting_point          415
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.897(2)
_cell_length_b                   11.357(2)
_cell_length_c                   21.303(4)
_cell_angle_alpha                90.045(6)
_cell_angle_beta                 101.926(5)
_cell_angle_gamma                113.572(6)
_cell_volume                     2138.1(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.23
_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.975
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18471
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.379
_diffrn_reflns_theta_min         0.981
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6937
_reflns_number_total             7562
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.798
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         7562
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0758
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1348P)²+10.6428P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2054
_refine_ls_wR_factor_ref         0.2190
_refine_special_details          'Refined as a 2-component twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.706(2)
 0.294(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C36) \\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.005
Uanis(C36) = Uanis(C34)
4.a Ternary CH refined with riding coordinates:
 C24(H24), C15(H15), C27(H27), C12(H12)
4.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C21(H21), C10(H10), C2(H2), C8(H8), C9(H9), C20(H20)
4.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C29(H29A,H29B,
 H29C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C14(H14A,H14B,H14C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C42(H42A,H42B,H42C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C13(H13A,H13B,
 H13C), C40(H40A,H40B,H40C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb Nb 0.07584(8) 0.25224(7) 0.27075(3) 0.01419(19) Uani 1 1 d . . . . .
C1 C 0.2604(8) 0.0852(7) 0.2647(4) 0.0170(15) Uani 1 1 d . . . . .
O1 O 0.2239(6) 0.2905(5) 0.1600(3) 0.0202(12) Uani 1 1 d . . . . .
C34 C 0.0816(11) 0.5222(8) 0.2206(4) 0.0275(13) Uani 1 1 d . . . . .
N4 N 0.1129(7) 0.4050(6) 0.2139(3) 0.0173(13) Uani 1 1 d . . . . .
O2 O 0.3062(7) 0.5064(6) 0.1480(3) 0.0309(14) Uani 1 1 d . . . . .
C36 C 0.1933(10) 0.6236(7) 0.2693(4) 0.0275(13) Uani 1 1 d . U . . .
H36A H 0.206733 0.587150 0.310666 0.041 Uiso 1 1 calc GR . . . .
H36B H 0.158141 0.691784 0.273857 0.041 Uiso 1 1 calc GR . . . .
H36C H 0.290045 0.659773 0.256172 0.041 Uiso 1 1 calc GR . . . .
N2 N -0.0481(7) 0.0703(6) 0.1999(3) 0.0165(13) Uani 1 1 d . . . . .
C3 C 0.0149(9) -0.0013(8) 0.1804(4) 0.0188(16) Uani 1 1 d . . . . .
C25 C -0.3420(9) -0.0969(8) 0.3221(4) 0.0237(17) Uani 1 1 d . . . . .
H25A H -0.337961 -0.009547 0.326461 0.036 Uiso 1 1 calc GR . . . .
H25B H -0.298261 -0.117809 0.363910 0.036 Uiso 1 1 calc GR . . . .
H25C H -0.447577 -0.158809 0.307462 0.036 Uiso 1 1 calc GR . . . .
C24 C -0.2517(8) -0.1039(7) 0.2727(4) 0.0187(14) Uani 1 1 d . . . . .
H24 H -0.143913 -0.041950 0.289155 0.022 Uiso 1 1 calc R . . . .
N1 N 0.2277(7) 0.1589(6) 0.3027(3) 0.0153(13) Uani 1 1 d . . . . .
C18 C -0.2110(9) 0.0244(7) 0.1754(3) 0.0163(15) Uani 1 1 d . . . . .
C33 C -0.1099(9) 0.2539(8) 0.4088(4) 0.0221(17) Uani 1 1 d . . . . .
H33A H -0.176575 0.270788 0.372537 0.033 Uiso 1 1 calc GR . . . .
H33B H -0.135011 0.270209 0.449202 0.033 Uiso 1 1 calc GR . . . .
H33C H -0.123754 0.163725 0.403796 0.033 Uiso 1 1 calc GR . . . .
C15 C 0.1411(10) -0.0485(8) 0.3875(4) 0.0246(18) Uani 1 1 d . . . . .
H15 H 0.099382 -0.050504 0.340334 0.030 Uiso 1 1 calc R . . . .
C29 C -0.2299(12) 0.2660(10) 0.0586(5) 0.035(2) Uani 1 1 d . . . . .
H29A H -0.324856 0.223809 0.026197 0.053 Uiso 1 1 calc GR . . . .
H29B H -0.156170 0.333607 0.039627 0.053 Uiso 1 1 calc GR . . . .
H29C H -0.248633 0.304394 0.095310 0.053 Uiso 1 1 calc GR . . . .
C22 C -0.4249(9) 0.0129(9) 0.0938(4) 0.0264(19) Uani 1 1 d . . . . .
H22 H -0.465076 0.041671 0.055388 0.032 Uiso 1 1 calc R . . . .
C21 C -0.5230(10) -0.0809(9) 0.1234(4) 0.0272(18) Uani 1 1 d . . . . .
H21 H -0.628491 -0.119191 0.104741 0.033 Uiso 1 1 calc R . . . .
N3 N 0.0889(7) 0.3191(6) 0.3486(3) 0.0169(13) Uani 1 1 d . . . . .
C41 C 0.3029(11) 0.2124(10) 0.0750(5) 0.033(2) Uani 1 1 d . . . . .
H41A H 0.294352 0.133800 0.095967 0.050 Uiso 1 1 calc GR . . . .
H41B H 0.381004 0.234083 0.049962 0.050 Uiso 1 1 calc GR . . . .
H41C H 0.205656 0.198229 0.046181 0.050 Uiso 1 1 calc GR . . . .
C43 C 0.5088(12) 0.5464(12) 0.0935(5) 0.047(3) Uani 1 1 d . . . . .
H43A H 0.504898 0.629145 0.082920 0.071 Uiso 1 1 calc GR . . . .
H43B H 0.539850 0.512638 0.059285 0.071 Uiso 1 1 calc GR . . . .
H43C H 0.581864 0.558972 0.134432 0.071 Uiso 1 1 calc GR . . . .
C11 C 0.2743(9) 0.0794(8) 0.4097(4) 0.0210(17) Uani 1 1 d . . . . .
C14 C 0.4863(10) 0.5334(8) 0.3776(4) 0.0251(18) Uani 1 1 d . . . . .
H14A H 0.563034 0.566027 0.418069 0.038 Uiso 1 1 calc GR . . . .
H14B H 0.385943 0.512735 0.385997 0.038 Uiso 1 1 calc GR . . . .
H14C H 0.507024 0.599276 0.347041 0.038 Uiso 1 1 calc GR . . . .
C31 C 0.0785(10) 0.4843(8) 0.4182(4) 0.0239(18) Uani 1 1 d . . . . .
H31A H 0.177920 0.540222 0.410753 0.036 Uiso 1 1 calc GR . . . .
H31B H 0.073040 0.505573 0.461901 0.036 Uiso 1 1 calc GR . . . .
H31C H -0.000675 0.497567 0.386855 0.036 Uiso 1 1 calc GR . . . .
C27 C -0.1676(9) 0.1661(8) 0.0815(4) 0.0216(17) Uani 1 1 d . . . . .
H27 H -0.066081 0.212138 0.111258 0.026 Uiso 1 1 calc R . . . .
C38 C 0.3455(9) 0.3219(9) 0.1255(4) 0.0234(17) Uani 1 1 d . . . . .
C32 C 0.1627(10) 0.3184(8) 0.4656(4) 0.0241(18) Uani 1 1 d . . . . .
H32A H 0.145811 0.227362 0.461777 0.036 Uiso 1 1 calc GR . . . .
H32B H 0.143660 0.339346 0.506677 0.036 Uiso 1 1 calc GR . . . .
H32C H 0.267495 0.372609 0.464022 0.036 Uiso 1 1 calc GR . . . .
C10 C 0.3611(10) 0.1012(9) 0.4726(4) 0.0250(18) Uani 1 1 d . . . . .
H10 H 0.336419 0.034103 0.500368 0.030 Uiso 1 1 calc R . . . .
C7 C 0.4379(9) 0.2999(8) 0.3915(4) 0.0188(16) Uani 1 1 d . . . . .
C28 C -0.1465(11) 0.1027(9) 0.0221(4) 0.030(2) Uani 1 1 d . . . . .
H28A H -0.100164 0.042561 0.036187 0.045 Uiso 1 1 calc GR . . . .
H28B H -0.080831 0.169588 -0.000200 0.045 Uiso 1 1 calc GR . . . .
H28C H -0.245288 0.055646 -0.007179 0.045 Uiso 1 1 calc GR . . . .
C26 C -0.2567(11) -0.2424(8) 0.2672(5) 0.0321(19) Uani 1 1 d . . . . .
H26A H -0.361242 -0.304426 0.250143 0.048 Uiso 1 1 calc GR . . . .
H26B H -0.218767 -0.263816 0.309957 0.048 Uiso 1 1 calc GR . . . .
H26C H -0.193301 -0.246055 0.238184 0.048 Uiso 1 1 calc GR . . . .
C16 C 0.0187(10) -0.0638(8) 0.4233(4) 0.0270(18) Uani 1 1 d . . . . .
H16A H 0.061703 -0.051518 0.469846 0.041 Uiso 1 1 calc GR . . . .
H16B H -0.062591 -0.150485 0.411989 0.041 Uiso 1 1 calc GR . . . .
H16C H -0.022238 0.000681 0.411364 0.041 Uiso 1 1 calc GR . . . .
C2 C 0.1646(9) 0.0162(8) 0.2057(4) 0.0199(16) Uani 1 1 d . . . . .
H2 H 0.206802 -0.022824 0.180389 0.024 Uiso 1 1 calc R . . . .
C8 C 0.5199(10) 0.3162(9) 0.4552(4) 0.0237(17) Uani 1 1 d . . . . .
H8 H 0.603105 0.395981 0.471186 0.028 Uiso 1 1 calc R . . . .
C30 C 0.0556(9) 0.3432(8) 0.4103(4) 0.0196(16) Uani 1 1 d . . . . .
C12 C 0.4908(9) 0.4111(8) 0.3491(4) 0.0224(17) Uani 1 1 d . . . . .
H12 H 0.421084 0.385044 0.305404 0.027 Uiso 1 1 calc R . . . .
C17 C 0.1894(11) -0.1622(9) 0.3987(4) 0.033(2) Uani 1 1 d . . . . .
H17A H 0.265701 -0.154284 0.374145 0.049 Uiso 1 1 calc GR . . . .
H17B H 0.100958 -0.243940 0.384329 0.049 Uiso 1 1 calc GR . . . .
H17C H 0.232076 -0.160335 0.444668 0.049 Uiso 1 1 calc GR . . . .
C42 C 0.2352(12) 0.4316(11) 0.0359(4) 0.040(2) Uani 1 1 d . . . . .
H42A H 0.136649 0.366521 0.039736 0.061 Uiso 1 1 calc GR . . . .
H42B H 0.267295 0.402523 0.000522 0.061 Uiso 1 1 calc GR . . . .
H42C H 0.226814 0.513378 0.027057 0.061 Uiso 1 1 calc GR . . . .
C9 C 0.4810(10) 0.2167(9) 0.4955(4) 0.0252(18) Uani 1 1 d . . . . .
H9 H 0.537544 0.228977 0.538678 0.030 Uiso 1 1 calc R . . . .
C23 C -0.2703(9) 0.0664(8) 0.1181(4) 0.0183(16) Uani 1 1 d . . . . .
C39 C 0.3531(11) 0.4511(9) 0.0996(4) 0.029(2) Uani 1 1 d . . . . .
C35 C 0.0609(13) 0.5790(10) 0.1557(4) 0.036(2) Uani 1 1 d . . . . .
H35A H 0.016805 0.641546 0.159006 0.055 Uiso 1 1 calc GR . . . .
H35B H -0.006718 0.509526 0.122187 0.055 Uiso 1 1 calc GR . . . .
H35C H 0.159421 0.622198 0.144628 0.055 Uiso 1 1 calc GR . . . .
C37 C -0.0693(10) 0.4790(9) 0.2404(4) 0.0263(18) Uani 1 1 d . . . . .
H37A H -0.063532 0.437716 0.280625 0.039 Uiso 1 1 calc GR . . . .
H37B H -0.149577 0.417275 0.206451 0.039 Uiso 1 1 calc GR . . . .
H37C H -0.091846 0.554074 0.246704 0.039 Uiso 1 1 calc GR . . . .
C5 C -0.0720(10) -0.1155(8) 0.1292(4) 0.0246(18) Uani 1 1 d . . . . .
H5A H -0.106363 -0.195648 0.150156 0.037 Uiso 1 1 calc GR . . . .
H5B H -0.005755 -0.118918 0.101466 0.037 Uiso 1 1 calc GR . . . .
H5C H -0.159811 -0.105184 0.103006 0.037 Uiso 1 1 calc GR . . . .
C20 C -0.4650(10) -0.1183(9) 0.1808(4) 0.0270(18) Uani 1 1 d . . . . .
H20 H -0.532156 -0.181209 0.202091 0.032 Uiso 1 1 calc R . . . .
C4 C 0.4067(10) 0.0666(9) 0.2847(4) 0.0270(19) Uani 1 1 d . . . . .
H4A H 0.490257 0.149612 0.302190 0.041 Uiso 1 1 calc GR . . . .
H4B H 0.427260 0.032802 0.247066 0.041 Uiso 1 1 calc GR . . . .
H4C H 0.396756 0.005420 0.317635 0.041 Uiso 1 1 calc GR . . . .
C13 C 0.6513(10) 0.4395(9) 0.3418(4) 0.0266(18) Uani 1 1 d . . . . .
H13A H 0.680595 0.506584 0.312199 0.040 Uiso 1 1 calc GR . . . .
H13B H 0.654178 0.360805 0.324506 0.040 Uiso 1 1 calc GR . . . .
H13C H 0.721782 0.469464 0.383948 0.040 Uiso 1 1 calc GR . . . .
C6 C 0.3152(8) 0.1821(7) 0.3692(3) 0.0146(15) Uani 1 1 d . . . . .
C19 C -0.3106(9) -0.0658(7) 0.2082(4) 0.0192(16) Uani 1 1 d . . . . .
C40 C 0.4866(11) 0.3340(12) 0.1743(4) 0.039(2) Uani 1 1 d . . . . .
H40A H 0.528907 0.416720 0.200611 0.059 Uiso 1 1 calc GR . . . .
H40B H 0.561555 0.329606 0.151724 0.059 Uiso 1 1 calc GR . . . .
H40C H 0.460659 0.263307 0.202145 0.059 Uiso 1 1 calc GR . . . .
B B 0.2150(10) 0.4058(9) 0.1752(4) 0.0184(18) Uani 1 1 d . . . . .
H H -0.143(8) 0.183(7) 0.268(4) 0.006(16) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb N4 2.071(6) . ?
Nb N2 2.292(7) . ?
Nb N1 2.168(6) . ?
Nb N3 1.782(6) . ?
Nb H 1.97(7) . ?
C1 N1 1.335(10) . ?
C1 C2 1.416(12) . ?
C1 C4 1.520(10) . ?
O1 C38 1.463(9) . ?
O1 B 1.390(10) . ?
C34 N4 1.495(11) . ?
C34 C36 1.460(12) . ?
C34 C35 1.535(11) . ?
C34 C37 1.524(13) . ?
N4 B 1.428(11) . ?
O2 C39 1.451(10) . ?
O2 B 1.359(11) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
N2 C3 1.318(10) . ?
N2 C18 1.458(10) . ?
C3 C2 1.399(11) . ?
C3 C5 1.526(11) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C25 C24 1.536(11) . ?
C24 H24 1.0000 . ?
C24 C26 1.557(10) . ?
C24 C19 1.513(11) . ?
N1 C6 1.462(9) . ?
C18 C23 1.410(11) . ?
C18 C19 1.410(11) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C33 C30 1.537(11) . ?
C15 H15 1.0000 . ?
C15 C11 1.510(13) . ?
C15 C16 1.516(12) . ?
C15 C17 1.549(12) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C29 C27 1.530(12) . ?
C22 H22 0.9500 . ?
C22 C21 1.380(13) . ?
C22 C23 1.382(11) . ?
C21 H21 0.9500 . ?
C21 C20 1.382(12) . ?
N3 C30 1.470(9) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C41 C38 1.508(12) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C43 C39 1.520(13) . ?
C11 C10 1.396(11) . ?
C11 C6 1.427(11) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C14 C12 1.536(11) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C31 C30 1.530(11) . ?
C27 H27 1.0000 . ?
C27 C28 1.546(11) . ?
C27 C23 1.527(11) . ?
C38 C39 1.547(13) . ?
C38 C40 1.516(12) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C32 C30 1.520(11) . ?
C10 H10 0.9500 . ?
C10 C9 1.371(13) . ?
C7 C8 1.398(11) . ?
C7 C12 1.536(12) . ?
C7 C6 1.397(11) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C2 H2 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.398(12) . ?
C12 H12 1.0000 . ?
C12 C13 1.530(11) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C42 C39 1.546(13) . ?
C9 H9 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C20 H20 0.9500 . ?
C20 C19 1.390(12) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Nb N2 105.2(2) . . ?
N4 Nb N1 126.6(2) . . ?
N4 Nb H 104(2) . . ?
N2 Nb H 70(2) . . ?
N1 Nb N2 82.1(2) . . ?
N1 Nb H 127(2) . . ?
N3 Nb N4 104.8(3) . . ?
N3 Nb N2 143.6(3) . . ?
N3 Nb N1 96.2(3) . . ?
N3 Nb H 83(2) . . ?
N1 C1 C2 124.6(7) . . ?
N1 C1 C4 120.4(7) . . ?
C2 C1 C4 115.0(6) . . ?
B O1 C38 106.8(6) . . ?
N4 C34 C35 111.3(7) . . ?
N4 C34 C37 107.2(6) . . ?
C36 C34 N4 115.0(8) . . ?
C36 C34 C35 109.5(7) . . ?
C36 C34 C37 107.0(7) . . ?
C37 C34 C35 106.3(8) . . ?
C34 N4 Nb 129.2(5) . . ?
B N4 Nb 109.8(5) . . ?
B N4 C34 119.0(6) . . ?
B O2 C39 106.6(7) . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C3 N2 Nb 125.4(5) . . ?
C3 N2 C18 115.6(7) . . ?
C18 N2 Nb 119.0(4) . . ?
N2 C3 C2 123.8(7) . . ?
N2 C3 C5 122.5(7) . . ?
C2 C3 C5 113.6(7) . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
C25 C24 H24 108.2 . . ?
C25 C24 C26 108.9(7) . . ?
C26 C24 H24 108.2 . . ?
C19 C24 C25 111.3(6) . . ?
C19 C24 H24 108.2 . . ?
C19 C24 C26 111.9(7) . . ?
C1 N1 Nb 125.2(5) . . ?
C1 N1 C6 113.6(6) . . ?
C6 N1 Nb 121.0(4) . . ?
C23 C18 N2 120.7(7) . . ?
C19 C18 N2 119.7(7) . . ?
C19 C18 C23 119.6(7) . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
C11 C15 H15 108.8 . . ?
C11 C15 C16 109.9(7) . . ?
C11 C15 C17 111.1(7) . . ?
C16 C15 H15 108.8 . . ?
C16 C15 C17 109.4(7) . . ?
C17 C15 H15 108.8 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
C21 C22 H22 119.0 . . ?
C21 C22 C23 122.1(8) . . ?
C23 C22 H22 119.0 . . ?
C22 C21 H21 120.6 . . ?
C22 C21 C20 118.8(8) . . ?
C20 C21 H21 120.6 . . ?
C30 N3 Nb 163.2(6) . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C39 C43 H43A 109.5 . . ?
C39 C43 H43B 109.5 . . ?
C39 C43 H43C 109.5 . . ?
C10 C11 C15 119.8(8) . . ?
C10 C11 C6 117.5(8) . . ?
C6 C11 C15 122.7(7) . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
C29 C27 H27 108.3 . . ?
C29 C27 C28 108.2(7) . . ?
C28 C27 H27 108.3 . . ?
C23 C27 C29 111.6(7) . . ?
C23 C27 H27 108.3 . . ?
C23 C27 C28 111.9(7) . . ?
O1 C38 C41 108.5(7) . . ?
O1 C38 C39 101.5(6) . . ?
O1 C38 C40 107.1(6) . . ?
C41 C38 C39 115.6(7) . . ?
C41 C38 C40 109.4(8) . . ?
C40 C38 C39 113.9(8) . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
C11 C10 H10 119.0 . . ?
C9 C10 C11 122.0(8) . . ?
C9 C10 H10 119.0 . . ?
C8 C7 C12 118.1(7) . . ?
C6 C7 C8 118.5(7) . . ?
C6 C7 C12 123.3(7) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1 C2 H2 116.2 . . ?
C3 C2 C1 127.6(7) . . ?
C3 C2 H2 116.2 . . ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.9(8) . . ?
C9 C8 H8 119.6 . . ?
N3 C30 C33 108.3(6) . . ?
N3 C30 C31 108.6(6) . . ?
N3 C30 C32 109.9(6) . . ?
C31 C30 C33 109.9(7) . . ?
C32 C30 C33 111.0(7) . . ?
C32 C30 C31 109.1(7) . . ?
C14 C12 H12 108.6 . . ?
C7 C12 C14 110.8(6) . . ?
C7 C12 H12 108.6 . . ?
C13 C12 C14 109.8(7) . . ?
C13 C12 C7 110.6(6) . . ?
C13 C12 H12 108.6 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
C10 C9 C8 119.8(7) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C18 C23 C27 121.7(7) . . ?
C22 C23 C18 118.9(8) . . ?
C22 C23 C27 119.4(7) . . ?
O2 C39 C43 108.4(8) . . ?
O2 C39 C38 102.9(6) . . ?
O2 C39 C42 106.2(7) . . ?
C43 C39 C38 115.6(8) . . ?
C43 C39 C42 110.4(8) . . ?
C42 C39 C38 112.6(8) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C21 C20 H20 119.2 . . ?
C21 C20 C19 121.5(8) . . ?
C19 C20 H20 119.3 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C6 N1 117.9(7) . . ?
C7 C6 N1 120.7(7) . . ?
C7 C6 C11 121.3(7) . . ?
C18 C19 C24 120.9(7) . . ?
C20 C19 C24 120.1(7) . . ?
C20 C19 C18 119.0(7) . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O1 B N4 118.7(7) . . ?
O2 B O1 112.6(7) . . ?
O2 B N4 128.7(7) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.706(2)
2 0.294(2)

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexamethyldisiloxane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 2004311'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-17 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'hydrido-(N-(tert-butyl)-1-phenylsilyl)amino-(tert-butyl)imino-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V) hexamethyldisiloxane solvate'
_chemical_name_common            (BDI)NbH(N[SiH2Ph]tBu)(NtBu)
_chemical_melting_point          393
_chemical_formula_moiety         'C43 H67 N4 Nb Si, C6 H18 O Si2'
_chemical_formula_sum            'C49 H85 N4 Nb O Si3'
_chemical_formula_weight         923.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6684(3)
_cell_length_b                   12.8523(4)
_cell_length_c                   21.1721(7)
_cell_angle_alpha                101.451(2)
_cell_angle_beta                 103.6950(10)
_cell_angle_gamma                103.1000(10)
_cell_volume                     2647.70(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9970
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      25.30

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_F_000             996
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.331
_shelx_estimated_absorpt_T_min   0.958
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6936
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            46576
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.688
_diffrn_reflns_theta_max         25.483
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9696
_reflns_number_gt                7258
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR-92
_computing_structure_refinement  SHELXL-2014
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0307P)²+3.5135P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9696
_refine_ls_number_parameters     557
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0476
_refine_ls_wR_factor_ref         0.0995
_refine_ls_wR_factor_gt          0.0880
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.2547(3) 0.4363(3) 0.73848(15) 0.0111(7) Uani 1 1 d . . . . .
C2 C -0.3372(3) 0.3263(3) 0.70766(15) 0.0130(7) Uani 1 1 d . . . . .
H2 H -0.4120 0.3036 0.7238 0.016 Uiso 1 1 calc R U . . .
C3 C -0.3232(3) 0.2471(3) 0.65682(16) 0.0124(7) Uani 1 1 d . . . . .
C4 C -0.3240(3) 0.5130(3) 0.77076(16) 0.0164(7) Uani 1 1 d . . . . .
H4A H -0.2565 0.5816 0.7997 0.025 Uiso 1 1 calc R U . . .
H4B H -0.3728 0.4767 0.7980 0.025 Uiso 1 1 calc R U . . .
H4C H -0.3875 0.5303 0.7355 0.025 Uiso 1 1 calc R U . . .
C5 C -0.4453(3) 0.1478(3) 0.62149(17) 0.0184(8) Uani 1 1 d . . . . .
H5A H -0.4426 0.1161 0.5759 0.028 Uiso 1 1 calc R U . . .
H5B H -0.5274 0.1710 0.6187 0.028 Uiso 1 1 calc R U . . .
H5C H -0.4450 0.0919 0.6470 0.028 Uiso 1 1 calc R U . . .
C6 C -0.0627(3) 0.5907(3) 0.76586(15) 0.0109(7) Uani 1 1 d . . . . .
C7 C -0.0023(3) 0.6354(3) 0.83578(15) 0.0129(7) Uani 1 1 d . . . . .
C8 C 0.0474(3) 0.7496(3) 0.86077(16) 0.0188(8) Uani 1 1 d . . . . .
H8 H 0.0871 0.7809 0.9080 0.023 Uiso 1 1 calc R U . . .
C9 C 0.0406(3) 0.8190(3) 0.81884(17) 0.0229(8) Uani 1 1 d . . . . .
H9 H 0.0726 0.8971 0.8372 0.027 Uiso 1 1 calc R U . . .
C10 C -0.0128(3) 0.7742(3) 0.75022(17) 0.0211(8) Uani 1 1 d . . . . .
H10 H -0.0148 0.8220 0.7213 0.025 Uiso 1 1 calc R U . . .
C11 C -0.0638(3) 0.6599(3) 0.72235(15) 0.0139(7) Uani 1 1 d . . . . .
C12 C 0.0099(3) 0.5647(3) 0.88474(16) 0.0169(7) Uani 1 1 d . . . . .
H12 H -0.0261 0.4852 0.8582 0.020 Uiso 1 1 calc R U . . .
C13 C -0.0714(3) 0.5848(3) 0.93427(17) 0.0272(9) Uani 1 1 d . . . . .
H13A H -0.0358 0.6618 0.9618 0.041 Uiso 1 1 calc R U . . .
H13B H -0.0643 0.5349 0.9636 0.041 Uiso 1 1 calc R U . . .
H13C H -0.1661 0.5705 0.9091 0.041 Uiso 1 1 calc R U . . .
C14 C 0.1578(3) 0.5857(3) 0.92443(17) 0.0243(8) Uani 1 1 d . . . . .
H14A H 0.2103 0.5738 0.8929 0.037 Uiso 1 1 calc R U . . .
H14B H 0.1638 0.5345 0.9529 0.037 Uiso 1 1 calc R U . . .
H14C H 0.1936 0.6622 0.9528 0.037 Uiso 1 1 calc R U . . .
C15 C -0.1223(3) 0.6151(3) 0.64628(15) 0.0157(7) Uani 1 1 d . . . . .
H15 H -0.1274 0.5346 0.6345 0.019 Uiso 1 1 calc R U . . .
C16 C -0.2657(3) 0.6243(3) 0.62270(18) 0.0264(9) Uani 1 1 d . . . . .
H16A H -0.3251 0.5760 0.6406 0.040 Uiso 1 1 calc R U . . .
H16B H -0.2981 0.6017 0.5733 0.040 Uiso 1 1 calc R U . . .
H16C H -0.2655 0.7012 0.6391 0.040 Uiso 1 1 calc R U . . .
C17 C -0.0323(4) 0.6725(3) 0.60973(17) 0.0237(8) Uani 1 1 d . . . . .
H17A H -0.0366 0.7489 0.6147 0.036 Uiso 1 1 calc R U . . .
H17B H -0.0632 0.6326 0.5618 0.036 Uiso 1 1 calc R U . . .
H17C H 0.0608 0.6728 0.6293 0.036 Uiso 1 1 calc R U . . .
C18 C -0.2209(3) 0.1895(2) 0.57223(15) 0.0109(7) Uani 1 1 d . . . . .
C19 C -0.2695(3) 0.2288(3) 0.51648(15) 0.0118(7) Uani 1 1 d . . . . .
C20 C -0.2846(3) 0.1654(3) 0.45211(16) 0.0175(8) Uani 1 1 d . . . . .
H20 H -0.3187 0.1906 0.4141 0.021 Uiso 1 1 calc R U . . .
C21 C -0.2517(3) 0.0673(3) 0.44208(17) 0.0197(8) Uani 1 1 d . . . . .
H21 H -0.2626 0.0253 0.3978 0.024 Uiso 1 1 calc R U . . .
C22 C -0.2022(3) 0.0306(3) 0.49758(17) 0.0179(8) Uani 1 1 d . . . . .
H22 H -0.1779 -0.0366 0.4908 0.022 Uiso 1 1 calc R U . . .
C23 C -0.1870(3) 0.0893(3) 0.56294(16) 0.0131(7) Uani 1 1 d . . . . .
C24 C -0.3088(3) 0.3362(3) 0.52332(16) 0.0149(7) Uani 1 1 d . . . . .
H24 H -0.2718 0.3792 0.5718 0.018 Uiso 1 1 calc R U . . .
C25 C -0.2475(3) 0.4069(3) 0.48185(17) 0.0232(8) Uani 1 1 d . . . . .
H25A H -0.1497 0.4198 0.4951 0.035 Uiso 1 1 calc R U . . .
H25B H -0.2680 0.4781 0.4901 0.035 Uiso 1 1 calc R U . . .
H25C H -0.2858 0.3680 0.4338 0.035 Uiso 1 1 calc R U . . .
C26 C -0.4618(3) 0.3155(3) 0.50273(19) 0.0269(9) Uani 1 1 d . . . . .
H26A H -0.5004 0.2743 0.4551 0.040 Uiso 1 1 calc R U . . .
H26B H -0.4825 0.3867 0.5095 0.040 Uiso 1 1 calc R U . . .
H26C H -0.5003 0.2724 0.5304 0.040 Uiso 1 1 calc R U . . .
C27 C -0.1386(3) 0.0402(3) 0.62030(16) 0.0157(7) Uani 1 1 d . . . . .
H27 H -0.1141 0.0985 0.6638 0.019 Uiso 1 1 calc R U . . .
C28 C -0.2511(4) -0.0584(3) 0.62069(19) 0.0272(9) Uani 1 1 d . . . . .
H28A H -0.3300 -0.0338 0.6249 0.041 Uiso 1 1 calc R U . . .
H28B H -0.2191 -0.0876 0.6589 0.041 Uiso 1 1 calc R U . . .
H28C H -0.2760 -0.1166 0.5785 0.041 Uiso 1 1 calc R U . . .
C29 C -0.0151(3) 0.0008(3) 0.61638(17) 0.0202(8) Uani 1 1 d . . . . .
H29A H -0.0399 -0.0618 0.5764 0.030 Uiso 1 1 calc R U . . .
H29B H 0.0182 -0.0226 0.6569 0.030 Uiso 1 1 calc R U . . .
H29C H 0.0557 0.0616 0.6133 0.030 Uiso 1 1 calc R U . . .
C30 C -0.0437(3) 0.2206(3) 0.83460(16) 0.0188(8) Uani 1 1 d . . . . .
C31 C -0.0995(4) 0.0965(3) 0.80028(18) 0.0281(9) Uani 1 1 d . . . . .
H31A H -0.1859 0.0819 0.7661 0.042 Uiso 1 1 calc R U . . .
H31B H -0.1127 0.0562 0.8340 0.042 Uiso 1 1 calc R U . . .
H31C H -0.0357 0.0718 0.7787 0.042 Uiso 1 1 calc R U . . .
C32 C -0.1469(4) 0.2599(3) 0.86548(18) 0.0270(9) Uani 1 1 d . . . . .
H32A H -0.1085 0.3382 0.8907 0.041 Uiso 1 1 calc R U . . .
H32B H -0.1696 0.2156 0.8960 0.041 Uiso 1 1 calc R U . . .
H32C H -0.2285 0.2512 0.8294 0.041 Uiso 1 1 calc R U . . .
C33 C 0.0897(4) 0.2454(3) 0.88933(17) 0.0293(9) Uani 1 1 d . . . . .
H33A H 0.1543 0.2188 0.8692 0.044 Uiso 1 1 calc R U . . .
H33B H 0.0748 0.2078 0.9240 0.044 Uiso 1 1 calc R U . . .
H33C H 0.1255 0.3255 0.9098 0.044 Uiso 1 1 calc R U . . .
C34 C 0.1755(3) 0.3550(3) 0.63487(15) 0.0124(7) Uani 1 1 d . . . . .
C35 C 0.0808(3) 0.4252(3) 0.61631(16) 0.0156(7) Uani 1 1 d . . . . .
H35A H -0.0125 0.3778 0.5989 0.023 Uiso 1 1 calc R U . . .
H35B H 0.1041 0.4596 0.5816 0.023 Uiso 1 1 calc R U . . .
H35C H 0.0905 0.4831 0.6565 0.023 Uiso 1 1 calc R U . . .
C36 C 0.1610(3) 0.2658(3) 0.57153(16) 0.0171(8) Uani 1 1 d . . . . .
H36A H 0.2193 0.2193 0.5833 0.026 Uiso 1 1 calc R U . . .
H36B H 0.1873 0.3013 0.5379 0.026 Uiso 1 1 calc R U . . .
H36C H 0.0671 0.2198 0.5529 0.026 Uiso 1 1 calc R U . . .
C37 C 0.3204(3) 0.4300(3) 0.66297(16) 0.0171(8) Uani 1 1 d . . . . .
H37A H 0.3293 0.4855 0.7041 0.026 Uiso 1 1 calc R U . . .
H37B H 0.3431 0.4674 0.6294 0.026 Uiso 1 1 calc R U . . .
H37C H 0.3817 0.3852 0.6734 0.026 Uiso 1 1 calc R U . . .
C38 C 0.3701(3) 0.3285(3) 0.80950(16) 0.0148(7) Uani 1 1 d . . . . .
C39 C 0.3715(3) 0.4350(3) 0.84135(16) 0.0178(8) Uani 1 1 d . . . . .
H39 H 0.3039 0.4657 0.8217 0.021 Uiso 1 1 calc R U . . .
C40 C 0.4694(3) 0.4968(3) 0.90095(17) 0.0212(8) Uani 1 1 d . . . . .
H40 H 0.4693 0.5697 0.9213 0.025 Uiso 1 1 calc R U . . .
C41 C 0.5667(3) 0.4530(3) 0.93070(17) 0.0246(9) Uani 1 1 d . . . . .
H41 H 0.6327 0.4948 0.9721 0.029 Uiso 1 1 calc R U . . .
C42 C 0.5684(3) 0.3481(3) 0.90041(17) 0.0254(9) Uani 1 1 d . . . . .
H42 H 0.6364 0.3181 0.9207 0.030 Uiso 1 1 calc R U . . .
C43 C 0.4717(3) 0.2866(3) 0.84080(17) 0.0233(8) Uani 1 1 d . . . . .
H43 H 0.4739 0.2144 0.8205 0.028 Uiso 1 1 calc R U . . .
C44 C -0.2749(5) 0.7793(4) 0.9092(2) 0.0541(13) Uani 1 1 d . . . . .
H44A H -0.3458 0.7105 0.8837 0.081 Uiso 1 1 calc R U . . .
H44B H -0.2201 0.7676 0.9500 0.081 Uiso 1 1 calc R U . . .
H44C H -0.2177 0.8010 0.8813 0.081 Uiso 1 1 calc R U . . .
C45 C -0.4599(6) 0.8453(4) 0.9858(3) 0.0716(16) Uani 1 1 d . . . . .
H45A H -0.4948 0.9058 1.0033 0.107 Uiso 1 1 calc R U . . .
H45B H -0.4064 0.8255 1.0235 0.107 Uiso 1 1 calc R U . . .
H45C H -0.5354 0.7807 0.9582 0.107 Uiso 1 1 calc R U . . .
C46 C -0.2242(6) 1.0191(4) 0.9789(3) 0.0719(16) Uani 1 1 d . . . . .
H46A H -0.1602 1.0348 0.9532 0.108 Uiso 1 1 calc R U . . .
H46B H -0.1765 1.0129 1.0231 0.108 Uiso 1 1 calc R U . . .
H46C H -0.2659 1.0794 0.9853 0.108 Uiso 1 1 calc R U . . .
C47 C -0.4387(5) 0.8061(4) 0.7339(2) 0.0553(13) Uani 1 1 d . . . . .
H47A H -0.3768 0.8731 0.7312 0.083 Uiso 1 1 calc R U . . .
H47B H -0.4985 0.7650 0.6887 0.083 Uiso 1 1 calc R U . . .
H47C H -0.3869 0.7595 0.7524 0.083 Uiso 1 1 calc R U . . .
C48 C -0.6622(4) 0.7191(3) 0.7903(2) 0.0470(12) Uani 1 1 d . . . . .
H48A H -0.6134 0.6693 0.8071 0.071 Uiso 1 1 calc R U . . .
H48B H -0.7215 0.6819 0.7444 0.071 Uiso 1 1 calc R U . . .
H48C H -0.7163 0.7387 0.8198 0.071 Uiso 1 1 calc R U . . .
C49 C -0.6308(5) 0.9424(4) 0.7591(3) 0.0637(15) Uani 1 1 d . . . . .
H49A H -0.6769 0.9682 0.7913 0.095 Uiso 1 1 calc R U . . .
H49B H -0.6970 0.9040 0.7150 0.095 Uiso 1 1 calc R U . . .
H49C H -0.5658 1.0061 0.7548 0.095 Uiso 1 1 calc R U . . .
N1 N -0.1277(2) 0.4716(2) 0.73856(12) 0.0086(6) Uani 1 1 d . . . . .
N2 N -0.2088(2) 0.2546(2) 0.63884(12) 0.0104(6) Uani 1 1 d . . . . .
N3 N -0.0215(2) 0.2796(2) 0.78368(13) 0.0135(6) Uani 1 1 d . . . . .
N4 N 0.1336(2) 0.3016(2) 0.68637(12) 0.0106(6) Uani 1 1 d . . . . .
Si1 Si 0.23748(8) 0.23727(8) 0.73082(4) 0.0134(2) Uani 1 1 d . . . . .
Si2 Si -0.35280(13) 0.89067(10) 0.93350(6) 0.0403(3) Uani 1 1 d . . . . .
Si3 Si -0.54087(12) 0.84574(9) 0.78966(6) 0.0344(3) Uani 1 1 d . . . . .
Nb Nb -0.01508(3) 0.34491(2) 0.71895(2) 0.00912(9) Uani 1 1 d . . . . .
O1 O -0.4447(3) 0.9092(2) 0.86562(14) 0.0484(8) Uani 1 1 d . . . . .
H1 H 0.105(3) 0.470(2) 0.7664(14) 0.014(8) Uiso 1 1 d . . . . .
H1A H 0.160(3) 0.150(2) 0.7458(14) 0.009(8) Uiso 1 1 d . . . . .
H1B H 0.308(3) 0.189(2) 0.6891(14) 0.015(8) Uiso 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.328(4) . ?
C1 C2 1.413(4) . ?
C1 C4 1.512(4) . ?
C2 C3 1.388(4) . ?
C2 H2 0.9500 . ?
C3 N2 1.351(4) . ?
C3 C5 1.514(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C11 1.401(4) . ?
C6 C7 1.407(4) . ?
C6 N1 1.461(4) . ?
C7 C8 1.386(5) . ?
C7 C12 1.510(4) . ?
C8 C9 1.379(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.376(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.394(5) . ?
C10 H10 0.9500 . ?
C11 C15 1.519(4) . ?
C12 C13 1.531(4) . ?
C12 C14 1.535(4) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.524(4) . ?
C15 C16 1.532(4) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C23 1.405(4) . ?
C18 C19 1.408(4) . ?
C18 N2 1.450(4) . ?
C19 C20 1.394(4) . ?
C19 C24 1.520(4) . ?
C20 C21 1.374(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.386(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.391(4) . ?
C22 H22 0.9500 . ?
C23 C27 1.514(4) . ?
C24 C25 1.531(4) . ?
C24 C26 1.532(4) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C29 1.530(4) . ?
C27 C28 1.538(4) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N3 1.468(4) . ?
C30 C31 1.527(5) . ?
C30 C33 1.529(5) . ?
C30 C32 1.535(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 N4 1.500(4) . ?
C34 C37 1.528(4) . ?
C34 C36 1.532(4) . ?
C34 C35 1.534(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.395(5) . ?
C38 C43 1.404(4) . ?
C38 Si1 1.873(3) . ?
C39 C40 1.384(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.374(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.379(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.378(5) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 Si2 1.858(4) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 Si2 1.850(5) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 Si2 1.803(5) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 Si3 1.861(4) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 Si3 1.840(4) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 Si3 1.857(5) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
N1 Nb 2.263(2) . ?
N2 Nb 2.228(2) . ?
N3 Nb 1.750(3) . ?
N4 Si1 1.740(3) . ?
N4 Nb 2.017(2) . ?
Si1 H1A 1.38(3) . ?
Si1 H1B 1.43(3) . ?
Si2 O1 1.630(3) . ?
Si3 O1 1.619(3) . ?
Nb H1 1.74(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.7(3) . . ?
N1 C1 C4 121.9(3) . . ?
C2 C1 C4 114.4(3) . . ?
C3 C2 C1 128.4(3) . . ?
C3 C2 H2 115.8 . . ?
C1 C2 H2 115.8 . . ?
N2 C3 C2 123.7(3) . . ?
N2 C3 C5 120.3(3) . . ?
C2 C3 C5 116.0(3) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C11 C6 C7 120.5(3) . . ?
C11 C6 N1 119.7(3) . . ?
C7 C6 N1 119.8(3) . . ?
C8 C7 C6 118.3(3) . . ?
C8 C7 C12 118.6(3) . . ?
C6 C7 C12 123.0(3) . . ?
C9 C8 C7 121.7(3) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C10 C9 C8 119.4(3) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 121.3(3) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C6 118.6(3) . . ?
C10 C11 C15 119.0(3) . . ?
C6 C11 C15 122.4(3) . . ?
C7 C12 C13 112.1(3) . . ?
C7 C12 C14 111.0(3) . . ?
C13 C12 C14 109.3(3) . . ?
C7 C12 H12 108.1 . . ?
C13 C12 H12 108.1 . . ?
C14 C12 H12 108.1 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C17 111.6(3) . . ?
C11 C15 C16 110.9(3) . . ?
C17 C15 C16 111.1(3) . . ?
C11 C15 H15 107.7 . . ?
C17 C15 H15 107.7 . . ?
C16 C15 H15 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C23 C18 C19 120.5(3) . . ?
C23 C18 N2 121.4(3) . . ?
C19 C18 N2 118.1(3) . . ?
C20 C19 C18 118.5(3) . . ?
C20 C19 C24 118.6(3) . . ?
C18 C19 C24 122.9(3) . . ?
C21 C20 C19 121.8(3) . . ?
C21 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C20 C21 C22 119.0(3) . . ?
C20 C21 H21 120.5 . . ?
C22 C21 H21 120.5 . . ?
C21 C22 C23 121.9(3) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 H22 119.1 . . ?
C22 C23 C18 118.4(3) . . ?
C22 C23 C27 118.3(3) . . ?
C18 C23 C27 123.3(3) . . ?
C19 C24 C25 111.2(3) . . ?
C19 C24 C26 112.2(3) . . ?
C25 C24 C26 109.7(3) . . ?
C19 C24 H24 107.9 . . ?
C25 C24 H24 107.9 . . ?
C26 C24 H24 107.9 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 C29 112.6(3) . . ?
C23 C27 C28 110.5(3) . . ?
C29 C27 C28 108.5(3) . . ?
C23 C27 H27 108.4 . . ?
C29 C27 H27 108.4 . . ?
C28 C27 H27 108.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 C31 108.8(3) . . ?
N3 C30 C33 109.3(3) . . ?
C31 C30 C33 110.5(3) . . ?
N3 C30 C32 108.8(3) . . ?
C31 C30 C32 109.3(3) . . ?
C33 C30 C32 110.1(3) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N4 C34 C37 111.2(2) . . ?
N4 C34 C36 109.9(2) . . ?
C37 C34 C36 110.0(2) . . ?
N4 C34 C35 107.5(2) . . ?
C37 C34 C35 109.1(3) . . ?
C36 C34 C35 109.0(3) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 C43 117.1(3) . . ?
C39 C38 Si1 124.1(2) . . ?
C43 C38 Si1 118.8(3) . . ?
C40 C39 C38 121.4(3) . . ?
C40 C39 H39 119.3 . . ?
C38 C39 H39 119.3 . . ?
C41 C40 C39 120.1(3) . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
C40 C41 C42 120.0(3) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C43 C42 C41 120.1(3) . . ?
C43 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
C42 C43 C38 121.3(3) . . ?
C42 C43 H43 119.3 . . ?
C38 C43 H43 119.3 . . ?
Si2 C44 H44A 109.5 . . ?
Si2 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
Si2 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Si2 C45 H45A 109.5 . . ?
Si2 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
Si2 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
Si2 C46 H46A 109.5 . . ?
Si2 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
Si2 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
Si3 C47 H47A 109.5 . . ?
Si3 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
Si3 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
Si3 C48 H48A 109.5 . . ?
Si3 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
Si3 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
Si3 C49 H49A 109.5 . . ?
Si3 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
Si3 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C1 N1 C6 116.2(2) . . ?
C1 N1 Nb 118.5(2) . . ?
C6 N1 Nb 123.88(17) . . ?
C3 N2 C18 117.1(2) . . ?
C3 N2 Nb 117.1(2) . . ?
C18 N2 Nb 125.07(17) . . ?
C30 N3 Nb 173.5(2) . . ?
C34 N4 Si1 120.09(19) . . ?
C34 N4 Nb 116.36(18) . . ?
Si1 N4 Nb 121.34(13) . . ?
N4 Si1 C38 116.21(14) . . ?
N4 Si1 H1A 109.6(11) . . ?
C38 Si1 H1A 109.5(11) . . ?
N4 Si1 H1B 110.1(11) . . ?
C38 Si1 H1B 105.7(12) . . ?
H1A Si1 H1B 105.1(16) . . ?
O1 Si2 C46 108.4(2) . . ?
O1 Si2 C45 109.9(2) . . ?
C46 Si2 C45 111.2(3) . . ?
O1 Si2 C44 109.27(19) . . ?
C46 Si2 C44 110.3(3) . . ?
C45 Si2 C44 107.7(2) . . ?
O1 Si3 C48 109.78(19) . . ?
O1 Si3 C49 107.3(2) . . ?
C48 Si3 C49 110.3(2) . . ?
O1 Si3 C47 110.4(2) . . ?
C48 Si3 C47 108.6(2) . . ?
C49 Si3 C47 110.4(2) . . ?
N3 Nb N4 102.81(11) . . ?
N3 Nb N2 103.99(11) . . ?
N4 Nb N2 107.50(9) . . ?
N3 Nb N1 103.08(10) . . ?
N4 Nb N1 149.17(9) . . ?
N2 Nb N1 82.03(9) . . ?
N3 Nb H1 98.6(9) . . ?
N4 Nb H1 87.0(9) . . ?
N2 Nb H1 149.3(9) . . ?
N1 Nb H1 72.8(9) . . ?
Si3 O1 Si2 143.37(19) . . ?

_refine_diff_density_max         1.117
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.091


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexamethyldisiloxane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bmkxr69
_database_code_depnum_ccdc_archive 'CCDC 2004138'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-14 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT602_bmkxr69             
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info  
RESPONSE: During the structure analysis, it was observed that the unit
cell contains large accessible voids, even after assigning electron
density peaks to diethyl ether solvent molecules. This affects the
diffraction pattern, mostly at low scattering angles. We were unable
to locate additional solvent molecules in the diffraction map. 
;
# end Validation Reply Form
_audit_creation_date             2020-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            (BDI)Nb(NAr)(N(tBu)CO2B(C6F5)3)
_chemical_name_systematic        
'(tris(pentafluorophenyl)borate-N-tert-butylcarbamidato-N,O)-(2,6-diisopropylphenyl)imino-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V) diethyl ether solvate'
_chemical_formula_moiety         'C64 H67 B F15 N4 Nb O2, C4 H10 O'
_chemical_formula_sum            'C68 H77 B F15 N4 Nb O3'
_chemical_formula_weight         1387.05
_chemical_melting_point          458
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.2228(19)
_cell_length_b                   24.338(2)
_cell_length_c                   24.561(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.576(3)
_cell_angle_gamma                90
_cell_volume                     13279(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.36
_shelx_estimated_absorpt_T_max   0.989
_shelx_estimated_absorpt_T_min   0.963
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             5744
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_av_unetI/netI     0.1368
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            63281
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.427
_diffrn_reflns_theta_min         1.659
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14154
_reflns_number_total             24250
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.938
_refine_diff_density_min         -1.594
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1695
_refine_ls_number_reflns         24250
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0688
_refine_ls_restrained_S_all      0.969
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0905P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1923
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C36(H36), C39(H39), C76(H76),
 C79(H79), C88(H88), C91(H91), C100(H100), C103(H103)
2.b Secondary CH2 refined with riding coordinates:
 C130(H13D,H13E), C131(H13F,H13G), C134(H13N,H13O), C135(H13P,H13Q)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32),
 C33(H33), C34(H34), C66(H66), C72(H72), C73(H73), C74(H74), C84(H84), C85(H85),
  C86(H86), C96(H96), C97(H97), C98(H98)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C80(H80A,H80B,H80C), C81(H81A,
 H81B,H81C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C92(H92A,H92B,H92C),
 C93(H93A,H93B,H93C), C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C104(H10G,
 H10H,H10I), C105(H10J,H10K,H10L), C107(H10M,H10N,H10O), C108(H10P,H10Q,H10R),
 C109(H10S,H10T,H10U), C129(H12A,H12B,H12C), C132(H13H,H13I,H13J), C133(H13K,
 H13L,H13M), C136(H13R,H13S,H13T)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3552(2) 0.7288(2) 0.8200(2) 0.0207(12) Uani 1 1 d . . . . .
C2 C 0.3703(2) 0.6920(2) 0.8607(2) 0.0232(13) Uani 1 1 d . . . . .
H2 H 0.342000 0.688627 0.888827 0.028 Uiso 1 1 calc R . . . .
C3 C 0.4220(2) 0.6588(2) 0.8664(2) 0.0204(12) Uani 1 1 d . . . . .
C4 C 0.2922(3) 0.7507(2) 0.8173(2) 0.0289(14) Uani 1 1 d . . . . .
H4A H 0.291061 0.786591 0.835387 0.043 Uiso 1 1 calc GR . . . .
H4B H 0.265429 0.725149 0.835738 0.043 Uiso 1 1 calc GR . . . .
H4C H 0.278919 0.754712 0.779167 0.043 Uiso 1 1 calc GR . . . .
C5 C 0.4198(3) 0.6157(2) 0.9101(2) 0.0300(14) Uani 1 1 d . . . . .
H5A H 0.416930 0.579241 0.893217 0.045 Uiso 1 1 calc GR . . . .
H5B H 0.384576 0.621904 0.932434 0.045 Uiso 1 1 calc GR . . . .
H5C H 0.456459 0.617701 0.933121 0.045 Uiso 1 1 calc GR . . . .
C6 C 0.3778(2) 0.7788(2) 0.7371(2) 0.0206(12) Uani 1 1 d . . . . .
C7 C 0.3705(2) 0.8357(2) 0.7448(2) 0.0208(13) Uani 1 1 d . . . . .
C8 C 0.3541(2) 0.8682(2) 0.7001(2) 0.0248(13) Uani 1 1 d . . . . .
H8 H 0.349420 0.906798 0.704334 0.030 Uiso 1 1 calc R . . . .
C9 C 0.3446(3) 0.8442(2) 0.6493(2) 0.0298(15) Uani 1 1 d . . . . .
H9 H 0.333401 0.866465 0.618938 0.036 Uiso 1 1 calc R . . . .
C10 C 0.3511(3) 0.7884(2) 0.6425(2) 0.0294(14) Uani 1 1 d . . . . .
H10 H 0.344177 0.773034 0.607313 0.035 Uiso 1 1 calc R . . . .
C11 C 0.3676(2) 0.7536(2) 0.6857(2) 0.0254(14) Uani 1 1 d . . . . .
C12 C 0.3774(2) 0.8638(2) 0.8006(2) 0.0207(13) Uani 1 1 d . . . . .
H12 H 0.383911 0.834496 0.828632 0.025 Uiso 1 1 calc R . . . .
C13 C 0.3194(2) 0.8954(2) 0.8147(2) 0.0247(13) Uani 1 1 d . . . . .
H13A H 0.322145 0.907495 0.852751 0.037 Uiso 1 1 calc GR . . . .
H13B H 0.284492 0.871165 0.809510 0.037 Uiso 1 1 calc GR . . . .
H13C H 0.314901 0.927455 0.790835 0.037 Uiso 1 1 calc GR . . . .
C14 C 0.4309(3) 0.9028(2) 0.8042(2) 0.0251(13) Uani 1 1 d . . . . .
H14A H 0.468075 0.882202 0.798363 0.038 Uiso 1 1 calc GR . . . .
H14B H 0.432856 0.920005 0.840236 0.038 Uiso 1 1 calc GR . . . .
H14C H 0.426258 0.931300 0.776161 0.038 Uiso 1 1 calc GR . . . .
C15 C 0.3721(2) 0.6926(2) 0.6778(2) 0.0246(13) Uani 1 1 d . . . . .
H15 H 0.409683 0.680064 0.697341 0.029 Uiso 1 1 calc R . . . .
C16 C 0.3181(3) 0.6617(2) 0.7039(3) 0.0358(16) Uani 1 1 d . . . . .
H16A H 0.316286 0.671396 0.742542 0.054 Uiso 1 1 calc GR . . . .
H16B H 0.323908 0.621931 0.700360 0.054 Uiso 1 1 calc GR . . . .
H16C H 0.280438 0.672387 0.685141 0.054 Uiso 1 1 calc GR . . . .
C17 C 0.3766(3) 0.6745(3) 0.6180(2) 0.0386(17) Uani 1 1 d . . . . .
H17A H 0.338978 0.683601 0.598211 0.058 Uiso 1 1 calc GR . . . .
H17B H 0.383399 0.634809 0.616451 0.058 Uiso 1 1 calc GR . . . .
H17C H 0.410138 0.693756 0.601348 0.058 Uiso 1 1 calc GR . . . .
C18 C 0.5104(2) 0.6151(2) 0.8409(2) 0.0190(12) Uani 1 1 d . . . . .
C19 C 0.4975(3) 0.5671(2) 0.8105(2) 0.0240(13) Uani 1 1 d . . . . .
C20 C 0.5315(3) 0.5200(2) 0.8224(2) 0.0250(13) Uani 1 1 d . . . . .
H20 H 0.523178 0.486938 0.803076 0.030 Uiso 1 1 calc R . . . .
C21 C 0.5765(3) 0.5211(2) 0.8614(2) 0.0283(14) Uani 1 1 d . . . . .
H21 H 0.598260 0.488402 0.869732 0.034 Uiso 1 1 calc R . . . .
C22 C 0.5908(3) 0.5686(2) 0.8887(2) 0.0275(14) Uani 1 1 d . . . . .
H22 H 0.623649 0.568904 0.914331 0.033 Uiso 1 1 calc R . . . .
C23 C 0.5576(3) 0.6170(2) 0.8793(2) 0.0220(13) Uani 1 1 d . . . . .
C24 C 0.4479(3) 0.5652(2) 0.7663(2) 0.0308(15) Uani 1 1 d . . . . .
H24 H 0.436509 0.603723 0.756481 0.037 Uiso 1 1 calc R . . . .
C25 C 0.3917(3) 0.5352(4) 0.7845(3) 0.065(3) Uani 1 1 d . . . . .
H25A H 0.402953 0.498871 0.798681 0.097 Uiso 1 1 calc GR . . . .
H25B H 0.363502 0.530969 0.753421 0.097 Uiso 1 1 calc GR . . . .
H25C H 0.372582 0.556486 0.813133 0.097 Uiso 1 1 calc GR . . . .
C26 C 0.4699(3) 0.5371(3) 0.7161(3) 0.048(2) Uani 1 1 d . . . . .
H26A H 0.472565 0.497443 0.722576 0.072 Uiso 1 1 calc GR . . . .
H26B H 0.509809 0.551350 0.707467 0.072 Uiso 1 1 calc GR . . . .
H26C H 0.441795 0.544248 0.685482 0.072 Uiso 1 1 calc GR . . . .
C27 C 0.5734(3) 0.6693(2) 0.9105(2) 0.0249(13) Uani 1 1 d . . . . .
H27 H 0.539982 0.696241 0.903960 0.030 Uiso 1 1 calc R . . . .
C28 C 0.5800(3) 0.6599(3) 0.9726(2) 0.0363(16) Uani 1 1 d . . . . .
H28A H 0.617564 0.640139 0.980801 0.054 Uiso 1 1 calc GR . . . .
H28B H 0.545858 0.638172 0.984973 0.054 Uiso 1 1 calc GR . . . .
H28C H 0.580720 0.695442 0.991360 0.054 Uiso 1 1 calc GR . . . .
C29 C 0.6306(3) 0.6944(2) 0.8895(2) 0.0268(14) Uani 1 1 d . . . . .
H29A H 0.664217 0.668975 0.895885 0.040 Uiso 1 1 calc GR . . . .
H29B H 0.638953 0.729073 0.908550 0.040 Uiso 1 1 calc GR . . . .
H29C H 0.625635 0.701483 0.850314 0.040 Uiso 1 1 calc GR . . . .
C30 C 0.5378(2) 0.8106(2) 0.8798(2) 0.0171(12) Uani 1 1 d . . . . .
C31 C 0.5945(2) 0.8367(2) 0.8753(2) 0.0199(12) Uani 1 1 d . . . . .
C32 C 0.6169(3) 0.8654(2) 0.9216(2) 0.0276(14) Uani 1 1 d . . . . .
H32 H 0.655339 0.882380 0.920194 0.033 Uiso 1 1 calc R . . . .
C33 C 0.5852(3) 0.8693(2) 0.9682(2) 0.0274(14) Uani 1 1 d . . . . .
H33 H 0.601307 0.889593 0.998264 0.033 Uiso 1 1 calc R . . . .
C34 C 0.5295(3) 0.8441(2) 0.9720(2) 0.0256(13) Uani 1 1 d . . . . .
H34 H 0.508236 0.846757 1.004940 0.031 Uiso 1 1 calc R . . . .
C35 C 0.5043(2) 0.8147(2) 0.9282(2) 0.0172(12) Uani 1 1 d . . . . .
C36 C 0.6302(2) 0.8379(2) 0.8244(2) 0.0233(13) Uani 1 1 d . . . . .
H36 H 0.610048 0.813082 0.797005 0.028 Uiso 1 1 calc R . . . .
C37 C 0.6289(3) 0.8975(2) 0.8012(2) 0.0292(14) Uani 1 1 d . . . . .
H37A H 0.586997 0.909651 0.796405 0.044 Uiso 1 1 calc GR . . . .
H37B H 0.648443 0.898123 0.765898 0.044 Uiso 1 1 calc GR . . . .
H37C H 0.650266 0.922169 0.826564 0.044 Uiso 1 1 calc GR . . . .
C38 C 0.6957(3) 0.8193(3) 0.8321(3) 0.0366(16) Uani 1 1 d . . . . .
H38A H 0.717032 0.844643 0.856863 0.055 Uiso 1 1 calc GR . . . .
H38B H 0.715169 0.819183 0.796766 0.055 Uiso 1 1 calc GR . . . .
H38C H 0.696766 0.782177 0.847530 0.055 Uiso 1 1 calc GR . . . .
C39 C 0.4425(2) 0.7905(2) 0.9347(2) 0.0216(13) Uani 1 1 d . . . . .
H39 H 0.430319 0.772657 0.899412 0.026 Uiso 1 1 calc R . . . .
C40 C 0.4423(3) 0.7458(2) 0.9791(2) 0.0290(14) Uani 1 1 d . . . . .
H40A H 0.471096 0.716969 0.970195 0.043 Uiso 1 1 calc GR . . . .
H40B H 0.401852 0.729952 0.981031 0.043 Uiso 1 1 calc GR . . . .
H40C H 0.453688 0.762204 1.014352 0.043 Uiso 1 1 calc GR . . . .
C41 C 0.3959(3) 0.8345(2) 0.9465(2) 0.0300(14) Uani 1 1 d . . . . .
H41A H 0.404691 0.850537 0.982498 0.045 Uiso 1 1 calc GR . . . .
H41B H 0.355702 0.818015 0.946013 0.045 Uiso 1 1 calc GR . . . .
H41C H 0.397503 0.863303 0.918734 0.045 Uiso 1 1 calc GR . . . .
C42 C 0.5492(2) 0.8008(2) 0.6742(2) 0.0189(12) Uani 1 1 d . . . . .
C43 C 0.5188(2) 0.8521(2) 0.6957(2) 0.0213(12) Uani 1 1 d . . . . .
H43A H 0.475689 0.845042 0.699354 0.032 Uiso 1 1 calc GR . . . .
H43B H 0.524439 0.882493 0.670169 0.032 Uiso 1 1 calc GR . . . .
H43C H 0.536720 0.861725 0.731290 0.032 Uiso 1 1 calc GR . . . .
C44 C 0.6168(2) 0.8117(2) 0.6698(2) 0.0236(13) Uani 1 1 d . . . . .
H44A H 0.635171 0.815076 0.706419 0.035 Uiso 1 1 calc GR . . . .
H44B H 0.622998 0.845913 0.649632 0.035 Uiso 1 1 calc GR . . . .
H44C H 0.635614 0.781179 0.650600 0.035 Uiso 1 1 calc GR . . . .
C45 C 0.5206(3) 0.7860(2) 0.6180(2) 0.0234(13) Uani 1 1 d . . . . .
H45A H 0.537033 0.750956 0.605618 0.035 Uiso 1 1 calc GR . . . .
H45B H 0.529772 0.814898 0.591745 0.035 Uiso 1 1 calc GR . . . .
H45C H 0.476864 0.782780 0.621131 0.035 Uiso 1 1 calc GR . . . .
C46 C 0.5639(2) 0.7068(2) 0.7118(2) 0.0154(11) Uani 1 1 d . . . . .
C47 C 0.6724(2) 0.6255(2) 0.7273(2) 0.0188(12) Uani 1 1 d . . . . .
C48 C 0.7078(2) 0.6638(2) 0.7554(2) 0.0201(12) Uani 1 1 d . . . . .
C49 C 0.7417(2) 0.6517(2) 0.8023(2) 0.0241(13) Uani 1 1 d . . . . .
C50 C 0.7397(3) 0.5994(3) 0.8225(2) 0.0282(14) Uani 1 1 d . . . . .
C51 C 0.7052(3) 0.5600(2) 0.7972(2) 0.0244(13) Uani 1 1 d . . . . .
C52 C 0.6712(2) 0.5743(2) 0.7511(2) 0.0199(12) Uani 1 1 d . . . . .
C53 C 0.6944(2) 0.6637(2) 0.6249(2) 0.0183(12) Uani 1 1 d . . . . .
C54 C 0.6761(2) 0.6897(2) 0.5765(2) 0.0206(12) Uani 1 1 d . . . . .
C55 C 0.7153(3) 0.7031(2) 0.5352(2) 0.0253(13) Uani 1 1 d . . . . .
C56 C 0.7740(3) 0.6883(2) 0.5399(2) 0.0260(14) Uani 1 1 d . . . . .
C57 C 0.7950(2) 0.6625(2) 0.5870(2) 0.0254(13) Uani 1 1 d . . . . .
C58 C 0.7547(2) 0.6511(2) 0.6275(2) 0.0197(12) Uani 1 1 d . . . . .
C59 C 0.6042(2) 0.5953(2) 0.6351(2) 0.0179(12) Uani 1 1 d . . . . .
C60 C 0.5454(3) 0.5982(2) 0.6170(2) 0.0228(13) Uani 1 1 d . . . . .
C61 C 0.5165(2) 0.5578(2) 0.5862(2) 0.0220(13) Uani 1 1 d . . . . .
C62 C 0.5481(3) 0.5118(2) 0.5718(2) 0.0246(14) Uani 1 1 d . . . . .
C63 C 0.6074(3) 0.5076(2) 0.5873(2) 0.0242(13) Uani 1 1 d . . . . .
C64 C 0.6342(2) 0.5486(2) 0.6178(2) 0.0191(12) Uani 1 1 d . . . . .
C65 C 1.1410(2) 0.5783(2) 0.1951(3) 0.0271(14) Uani 1 1 d . . . . .
C66 C 1.1269(2) 0.5417(2) 0.1535(2) 0.0252(14) Uani 1 1 d . . . . .
H66 H 1.155787 0.538460 0.125913 0.030 Uiso 1 1 calc R . . . .
C67 C 1.0761(2) 0.5095(2) 0.1470(2) 0.0206(12) Uani 1 1 d . . . . .
C68 C 1.2046(2) 0.6012(2) 0.1989(3) 0.0346(16) Uani 1 1 d . . . . .
H68A H 1.212143 0.617051 0.235076 0.052 Uiso 1 1 calc GR . . . .
H68B H 1.209346 0.629651 0.171107 0.052 Uiso 1 1 calc GR . . . .
H68C H 1.233492 0.571472 0.192798 0.052 Uiso 1 1 calc GR . . . .
C69 C 1.0793(3) 0.4669(2) 0.1019(2) 0.0254(13) Uani 1 1 d . . . . .
H69A H 1.081482 0.430092 0.117949 0.038 Uiso 1 1 calc GR . . . .
H69B H 1.115189 0.473542 0.080549 0.038 Uiso 1 1 calc GR . . . .
H69C H 1.043273 0.469736 0.078167 0.038 Uiso 1 1 calc GR . . . .
C70 C 1.1175(2) 0.6301(2) 0.2768(2) 0.0252(14) Uani 1 1 d . . . . .
C71 C 1.1248(2) 0.6863(2) 0.2670(2) 0.0235(13) Uani 1 1 d . . . . .
C72 C 1.1389(2) 0.7197(2) 0.3112(2) 0.0292(15) Uani 1 1 d . . . . .
H72 H 1.144323 0.757942 0.305349 0.035 Uiso 1 1 calc R . . . .
C73 C 1.1454(3) 0.6995(3) 0.3632(3) 0.0382(17) Uani 1 1 d . . . . .
H73 H 1.153650 0.723842 0.392694 0.046 Uiso 1 1 calc R . . . .
C74 C 1.1400(3) 0.6436(3) 0.3726(3) 0.0401(18) Uani 1 1 d . . . . .
H74 H 1.146871 0.629667 0.408363 0.048 Uiso 1 1 calc R . . . .
C75 C 1.1246(3) 0.6072(2) 0.3301(3) 0.0300(15) Uani 1 1 d . . . . .
C76 C 1.1187(2) 0.7124(2) 0.2109(2) 0.0246(13) Uani 1 1 d . . . . .
H76 H 1.111971 0.682376 0.183550 0.030 Uiso 1 1 calc R . . . .
C77 C 1.1763(3) 0.7436(2) 0.1962(3) 0.0288(14) Uani 1 1 d . . . . .
H77A H 1.182204 0.774754 0.221034 0.043 Uiso 1 1 calc GR . . . .
H77B H 1.172512 0.757025 0.158665 0.043 Uiso 1 1 calc GR . . . .
H77C H 1.210991 0.718779 0.199596 0.043 Uiso 1 1 calc GR . . . .
C78 C 1.0642(3) 0.7519(2) 0.2071(3) 0.0296(14) Uani 1 1 d . . . . .
H78A H 1.027020 0.731233 0.212418 0.044 Uiso 1 1 calc GR . . . .
H78B H 1.062607 0.769365 0.171093 0.044 Uiso 1 1 calc GR . . . .
H78C H 1.068557 0.780235 0.235276 0.044 Uiso 1 1 calc GR . . . .
C79 C 1.1193(3) 0.5451(3) 0.3405(3) 0.0413(19) Uani 1 1 d . . . . .
H79 H 1.082103 0.532007 0.320614 0.050 Uiso 1 1 calc R . . . .
C80 C 1.1725(3) 0.5144(3) 0.3173(3) 0.056(2) Uani 1 1 d . . . . .
H80A H 1.173559 0.520563 0.277879 0.084 Uiso 1 1 calc GR . . . .
H80B H 1.168334 0.475005 0.324493 0.084 Uiso 1 1 calc GR . . . .
H80C H 1.210003 0.527869 0.334522 0.084 Uiso 1 1 calc GR . . . .
C81 C 1.1128(3) 0.5305(3) 0.4010(3) 0.049(2) Uani 1 1 d . . . . .
H81A H 1.103117 0.491384 0.404420 0.074 Uiso 1 1 calc GR . . . .
H81B H 1.080397 0.552495 0.416344 0.074 Uiso 1 1 calc GR . . . .
H81C H 1.150673 0.538309 0.420871 0.074 Uiso 1 1 calc GR . . . .
C82 C 0.9870(2) 0.4653(2) 0.1709(2) 0.0167(12) Uani 1 1 d . . . . .
C83 C 0.9398(2) 0.4681(2) 0.1319(2) 0.0171(12) Uani 1 1 d . . . . .
C84 C 0.9085(3) 0.4198(2) 0.1199(2) 0.0221(12) Uani 1 1 d . . . . .
H84 H 0.875650 0.420893 0.094320 0.027 Uiso 1 1 calc R . . . .
C85 C 0.9240(3) 0.3703(2) 0.1441(2) 0.0244(13) Uani 1 1 d . . . . .
H85 H 0.903395 0.337439 0.134030 0.029 Uiso 1 1 calc R . . . .
C86 C 0.9700(3) 0.3693(2) 0.1833(2) 0.0255(14) Uani 1 1 d . . . . .
H86 H 0.980249 0.335241 0.200100 0.031 Uiso 1 1 calc R . . . .
C87 C 1.0019(2) 0.4163(2) 0.1990(2) 0.0221(12) Uani 1 1 d . . . . .
C88 C 0.9219(2) 0.5215(2) 0.1040(2) 0.0199(12) Uani 1 1 d . . . . .
H88 H 0.954523 0.548857 0.111929 0.024 Uiso 1 1 calc R . . . .
C89 C 0.9145(3) 0.5163(2) 0.0418(2) 0.0287(14) Uani 1 1 d . . . . .
H89A H 0.951046 0.500157 0.027076 0.043 Uiso 1 1 calc GR . . . .
H89B H 0.907801 0.552745 0.025895 0.043 Uiso 1 1 calc GR . . . .
H89C H 0.879973 0.492589 0.032858 0.043 Uiso 1 1 calc GR . . . .
C90 C 0.8637(3) 0.5440(2) 0.1274(2) 0.0264(14) Uani 1 1 d . . . . .
H90A H 0.831643 0.516517 0.123039 0.040 Uiso 1 1 calc GR . . . .
H90B H 0.851874 0.577614 0.107884 0.040 Uiso 1 1 calc GR . . . .
H90C H 0.870167 0.552272 0.166141 0.040 Uiso 1 1 calc GR . . . .
C91 C 1.0507(3) 0.4139(2) 0.2438(2) 0.0277(14) Uani 1 1 d . . . . .
H91 H 1.058529 0.452431 0.256250 0.033 Uiso 1 1 calc R . . . .
C92 C 1.0295(3) 0.3812(3) 0.2931(2) 0.0336(15) Uani 1 1 d . . . . .
H92A H 1.026924 0.342179 0.283638 0.050 Uiso 1 1 calc GR . . . .
H92B H 0.989739 0.394473 0.303427 0.050 Uiso 1 1 calc GR . . . .
H92C H 1.058208 0.386216 0.323666 0.050 Uiso 1 1 calc GR . . . .
C93 C 1.1098(3) 0.3909(3) 0.2239(3) 0.0461(19) Uani 1 1 d . . . . .
H93A H 1.102699 0.354779 0.207312 0.069 Uiso 1 1 calc GR . . . .
H93B H 1.138386 0.387158 0.254828 0.069 Uiso 1 1 calc GR . . . .
H93C H 1.126428 0.415865 0.196918 0.069 Uiso 1 1 calc GR . . . .
C94 C 0.9562(3) 0.6588(2) 0.1356(2) 0.0220(13) Uani 1 1 d . . . . .
C95 C 0.9894(3) 0.6637(2) 0.0873(2) 0.0274(14) Uani 1 1 d . . . . .
C96 C 0.9620(3) 0.6895(3) 0.0430(3) 0.0418(17) Uani 1 1 d . . . . .
H96 H 0.983468 0.692688 0.010249 0.050 Uiso 1 1 calc R . . . .
C97 C 0.9043(3) 0.7109(3) 0.0446(3) 0.051(2) Uani 1 1 d . . . . .
H97 H 0.886351 0.727745 0.013262 0.061 Uiso 1 1 calc R . . . .
C98 C 0.8734(3) 0.7076(3) 0.0921(3) 0.0395(17) Uani 1 1 d . . . . .
H98 H 0.833932 0.722368 0.093160 0.047 Uiso 1 1 calc R . . . .
C99 C 0.8986(3) 0.6828(2) 0.1396(2) 0.0267(14) Uani 1 1 d . . . . .
C100 C 1.0529(3) 0.6425(2) 0.0824(2) 0.0265(14) Uani 1 1 d . . . . .
H100 H 1.065993 0.626332 0.118202 0.032 Uiso 1 1 calc R . . . .
C101 C 1.0576(3) 0.5983(2) 0.0390(2) 0.0317(15) Uani 1 1 d . . . . .
H10A H 1.031039 0.567558 0.047653 0.047 Uiso 1 1 calc GR . . . .
H10B H 1.099278 0.585159 0.037861 0.047 Uiso 1 1 calc GR . . . .
H10C H 1.045631 0.613580 0.003390 0.047 Uiso 1 1 calc GR . . . .
C102 C 1.0964(3) 0.6899(2) 0.0688(3) 0.0373(16) Uani 1 1 d . . . . .
H10D H 1.088223 0.702503 0.031456 0.056 Uiso 1 1 calc GR . . . .
H10E H 1.138065 0.676796 0.072249 0.056 Uiso 1 1 calc GR . . . .
H10F H 1.090584 0.720404 0.094174 0.056 Uiso 1 1 calc GR . . . .
C103 C 0.8651(2) 0.6854(2) 0.1916(2) 0.0250(13) Uani 1 1 d . . . . .
H103 H 0.885751 0.660700 0.218806 0.030 Uiso 1 1 calc R . . . .
C104 C 0.8670(3) 0.7440(2) 0.2139(3) 0.0343(16) Uani 1 1 d . . . . .
H10G H 0.908383 0.757824 0.213588 0.051 Uiso 1 1 calc GR . . . .
H10H H 0.852703 0.744217 0.251287 0.051 Uiso 1 1 calc GR . . . .
H10I H 0.840991 0.767646 0.191043 0.051 Uiso 1 1 calc GR . . . .
C105 C 0.7982(3) 0.6677(2) 0.1859(3) 0.0348(16) Uani 1 1 d . . . . .
H10J H 0.776142 0.694079 0.162774 0.052 Uiso 1 1 calc GR . . . .
H10K H 0.780457 0.666722 0.222002 0.052 Uiso 1 1 calc GR . . . .
H10L H 0.795674 0.631091 0.169377 0.052 Uiso 1 1 calc GR . . . .
C106 C 0.9444(3) 0.6456(2) 0.3422(2) 0.0288(14) Uani 1 1 d . . . . .
C107 C 0.9712(3) 0.6313(3) 0.3976(2) 0.0393(17) Uani 1 1 d . . . . .
H10M H 0.953766 0.596748 0.410279 0.059 Uiso 1 1 calc GR . . . .
H10N H 0.962319 0.660713 0.423450 0.059 Uiso 1 1 calc GR . . . .
H10O H 1.014896 0.627181 0.395094 0.059 Uiso 1 1 calc GR . . . .
C108 C 0.8759(3) 0.6541(2) 0.3440(3) 0.0322(15) Uani 1 1 d . . . . .
H10P H 0.859283 0.658265 0.306883 0.048 Uiso 1 1 calc GR . . . .
H10Q H 0.867313 0.687273 0.365104 0.048 Uiso 1 1 calc GR . . . .
H10R H 0.857372 0.622246 0.361320 0.048 Uiso 1 1 calc GR . . . .
C109 C 0.9745(3) 0.6977(2) 0.3214(3) 0.0342(16) Uani 1 1 d . . . . .
H10S H 1.017753 0.691214 0.318226 0.051 Uiso 1 1 calc GR . . . .
H10T H 0.967991 0.727826 0.347046 0.051 Uiso 1 1 calc GR . . . .
H10U H 0.956973 0.707418 0.285639 0.051 Uiso 1 1 calc GR . . . .
C110 C 0.9341(2) 0.5511(2) 0.3036(2) 0.0170(12) Uani 1 1 d . . . . .
C111 C 0.8080(2) 0.5040(2) 0.3893(2) 0.0197(12) Uani 1 1 d . . . . .
C112 C 0.7462(3) 0.4961(2) 0.3861(2) 0.0218(13) Uani 1 1 d . . . . .
C113 C 0.7071(3) 0.5115(2) 0.4272(2) 0.0260(14) Uani 1 1 d . . . . .
C114 C 0.7300(3) 0.5347(2) 0.4734(2) 0.0248(13) Uani 1 1 d . . . . .
C115 C 0.7913(3) 0.5426(2) 0.4797(2) 0.0254(13) Uani 1 1 d . . . . .
C116 C 0.8280(2) 0.5262(2) 0.4387(2) 0.0216(13) Uani 1 1 d . . . . .
C117 C 0.8949(2) 0.4353(2) 0.3776(2) 0.0208(12) Uani 1 1 d . . . . .
C118 C 0.8628(3) 0.3900(2) 0.3966(2) 0.0236(13) Uani 1 1 d . . . . .
C119 C 0.8862(3) 0.3513(2) 0.4317(2) 0.0302(15) Uani 1 1 d . . . . .
C120 C 0.9455(3) 0.3557(2) 0.4497(3) 0.0361(17) Uani 1 1 d . . . . .
C121 C 0.9799(3) 0.3983(3) 0.4315(2) 0.0328(15) Uani 1 1 d . . . . .
C122 C 0.9543(3) 0.4369(2) 0.3966(2) 0.0261(14) Uani 1 1 d . . . . .
C123 C 0.8280(2) 0.4683(2) 0.2862(2) 0.0203(12) Uani 1 1 d . . . . .
C124 C 0.8304(2) 0.4181(2) 0.2603(2) 0.0221(13) Uani 1 1 d . . . . .
C125 C 0.7973(3) 0.4067(2) 0.2120(2) 0.0245(13) Uani 1 1 d . . . . .
C126 C 0.7629(3) 0.4454(2) 0.1880(2) 0.0233(13) Uani 1 1 d . . . . .
C127 C 0.7601(3) 0.4981(2) 0.2107(2) 0.0251(13) Uani 1 1 d . . . . .
C128 C 0.7925(2) 0.5074(2) 0.2584(2) 0.0200(12) Uani 1 1 d . . . . .
C129 C 0.7520(4) 0.2823(4) 1.0091(4) 0.071(3) Uani 1 1 d . . . . .
H12A H 0.708378 0.278211 1.003896 0.106 Uiso 1 1 calc GR . . . .
H12B H 0.766340 0.257835 1.038346 0.106 Uiso 1 1 calc GR . . . .
H12C H 0.771885 0.272682 0.975208 0.106 Uiso 1 1 calc GR . . . .
C130 C 0.7664(4) 0.3400(4) 1.0237(3) 0.067(2) Uani 1 1 d . . . . .
H13D H 0.752219 0.348494 1.060671 0.080 Uiso 1 1 calc R . . . .
H13E H 0.810439 0.346223 1.023304 0.080 Uiso 1 1 calc R . . . .
C131 C 0.7468(4) 0.4325(3) 0.9923(4) 0.072(3) Uani 1 1 d . . . . .
H13F H 0.790647 0.439638 0.991892 0.086 Uiso 1 1 calc R . . . .
H13G H 0.731956 0.443245 1.028375 0.086 Uiso 1 1 calc R . . . .
C132 C 0.7162(5) 0.4644(4) 0.9498(4) 0.096(4) Uani 1 1 d . . . . .
H13H H 0.735907 0.458439 0.915053 0.143 Uiso 1 1 calc GR . . . .
H13I H 0.717926 0.503482 0.959201 0.143 Uiso 1 1 calc GR . . . .
H13J H 0.674018 0.452716 0.946376 0.143 Uiso 1 1 calc GR . . . .
C133 C 0.5683(6) 0.5202(5) 1.0374(5) 0.168(8) Uani 1 1 d . . . . .
H13K H 0.561004 0.538100 1.002133 0.253 Uiso 1 1 calc GR . . . .
H13L H 0.531883 0.522448 1.058951 0.253 Uiso 1 1 calc GR . . . .
H13M H 0.578683 0.481524 1.031670 0.253 Uiso 1 1 calc GR . . . .
C134 C 0.6194(5) 0.5485(5) 1.0674(4) 0.108(4) Uani 1 1 d . . . . .
H13N H 0.603702 0.581710 1.085534 0.129 Uiso 1 1 calc R . . . .
H13O H 0.635615 0.523655 1.096146 0.129 Uiso 1 1 calc R . . . .
C135 C 0.7173(5) 0.5980(5) 1.0513(5) 0.128(5) Uani 1 1 d . . . . .
H13P H 0.738478 0.577498 1.080930 0.153 Uiso 1 1 calc R . . . .
H13Q H 0.699949 0.631289 1.067839 0.153 Uiso 1 1 calc R . . . .
C136 C 0.7637(6) 0.6163(6) 1.0118(5) 0.132(5) Uani 1 1 d . . . . .
H13R H 0.783786 0.584062 0.996759 0.198 Uiso 1 1 calc GR . . . .
H13S H 0.793500 0.639649 1.030677 0.198 Uiso 1 1 calc GR . . . .
H13T H 0.744013 0.637138 0.982160 0.198 Uiso 1 1 calc GR . . . .
B1 B 0.6419(3) 0.6438(2) 0.6683(3) 0.0181(14) Uani 1 1 d . . . . .
B2 B 0.8581(3) 0.4842(2) 0.3449(3) 0.0187(14) Uani 1 1 d . . . . .
N1 N 0.39600(19) 0.74376(17) 0.78248(17) 0.0163(10) Uani 1 1 d . . . . .
N2 N 0.46924(19) 0.66188(17) 0.83445(17) 0.0161(10) Uani 1 1 d . . . . .
N3 N 0.51448(19) 0.77876(17) 0.83510(17) 0.0165(10) Uani 1 1 d . . . . .
N4 N 0.53630(19) 0.75510(16) 0.71286(16) 0.0139(9) Uani 1 1 d . . . . .
N5 N 1.1004(2) 0.59357(18) 0.23202(19) 0.0242(11) Uani 1 1 d . . . . .
N6 N 1.02747(19) 0.51227(17) 0.17807(18) 0.0189(10) Uani 1 1 d . . . . .
N7 N 0.98080(19) 0.62859(17) 0.18092(17) 0.0171(10) Uani 1 1 d . . . . .
N8 N 0.95914(19) 0.60062(17) 0.30282(18) 0.0191(10) Uani 1 1 d . . . . .
O1 O 0.54842(15) 0.67411(14) 0.75094(13) 0.0158(8) Uani 1 1 d . . . . .
O2 O 0.60328(15) 0.69444(14) 0.67599(14) 0.0173(8) Uani 1 1 d . . . . .
O3 O 0.95029(16) 0.52008(14) 0.26265(14) 0.0189(8) Uani 1 1 d . . . . .
O4 O 0.89675(16) 0.53598(15) 0.33959(15) 0.0216(9) Uani 1 1 d . . . . .
O5 O 0.7353(3) 0.3753(2) 0.9828(2) 0.0653(16) Uani 1 1 d . . . . .
O6 O 0.6687(4) 0.5648(3) 1.0319(3) 0.112(3) Uani 1 1 d . . . . .
F1 F 0.71292(15) 0.71562(12) 0.73557(13) 0.0266(8) Uani 1 1 d . . . . .
F2 F 0.77534(15) 0.69073(13) 0.82719(13) 0.0337(9) Uani 1 1 d . . . . .
F3 F 0.77245(16) 0.58690(15) 0.86862(13) 0.0393(9) Uani 1 1 d . . . . .
F4 F 0.70433(16) 0.50899(13) 0.81752(13) 0.0354(9) Uani 1 1 d . . . . .
F5 F 0.63713(15) 0.53276(12) 0.73003(13) 0.0284(8) Uani 1 1 d . . . . .
F6 F 0.61791(14) 0.70346(13) 0.56761(12) 0.0269(8) Uani 1 1 d . . . . .
F7 F 0.69483(16) 0.72825(14) 0.48984(13) 0.0385(9) Uani 1 1 d . . . . .
F8 F 0.81165(15) 0.69829(15) 0.49937(14) 0.0398(9) Uani 1 1 d . . . . .
F9 F 0.85298(14) 0.64909(14) 0.59305(14) 0.0357(9) Uani 1 1 d . . . . .
F10 F 0.77930(14) 0.62408(13) 0.67139(12) 0.0265(8) Uani 1 1 d . . . . .
F11 F 0.51009(14) 0.64175(13) 0.63036(13) 0.0295(8) Uani 1 1 d . . . . .
F12 F 0.45771(14) 0.56297(14) 0.57187(13) 0.0348(9) Uani 1 1 d . . . . .
F13 F 0.52084(16) 0.47081(13) 0.54420(14) 0.0381(9) Uani 1 1 d . . . . .
F14 F 0.64039(16) 0.46433(12) 0.57092(13) 0.0335(9) Uani 1 1 d . . . . .
F15 F 0.69326(13) 0.54205(12) 0.63158(12) 0.0238(7) Uani 1 1 d . . . . .
F16 F 0.71893(14) 0.47276(12) 0.34173(13) 0.0261(8) Uani 1 1 d . . . . .
F17 F 0.64762(15) 0.50272(14) 0.42086(14) 0.0347(9) Uani 1 1 d . . . . .
F18 F 0.69338(16) 0.55193(14) 0.51309(14) 0.0398(9) Uani 1 1 d . . . . .
F19 F 0.81408(16) 0.56468(14) 0.52613(13) 0.0358(9) Uani 1 1 d . . . . .
F20 F 0.88773(15) 0.53197(13) 0.44952(13) 0.0306(8) Uani 1 1 d . . . . .
F21 F 0.80416(14) 0.38404(12) 0.38139(13) 0.0300(8) Uani 1 1 d . . . . .
F22 F 0.85168(17) 0.30941(14) 0.45021(15) 0.0461(10) Uani 1 1 d . . . . .
F23 F 0.96892(19) 0.31764(15) 0.48416(16) 0.0553(12) Uani 1 1 d . . . . .
F24 F 1.03733(17) 0.40324(16) 0.44810(16) 0.0501(11) Uani 1 1 d . . . . .
F25 F 0.99072(15) 0.47821(14) 0.38101(14) 0.0344(9) Uani 1 1 d . . . . .
F26 F 0.86365(14) 0.37671(12) 0.28068(13) 0.0288(8) Uani 1 1 d . . . . .
F27 F 0.80001(15) 0.35533(12) 0.18993(13) 0.0316(8) Uani 1 1 d . . . . .
F28 F 0.73266(15) 0.43497(14) 0.14071(13) 0.0354(9) Uani 1 1 d . . . . .
F29 F 0.72699(15) 0.53716(13) 0.18664(13) 0.0332(8) Uani 1 1 d . . . . .
F30 F 0.78737(15) 0.55863(12) 0.27970(12) 0.0267(8) Uani 1 1 d . . . . .
Nb1 Nb 0.48877(2) 0.73347(2) 0.78370(2) 0.01486(13) Uani 1 1 d . . . . .
Nb2 Nb 1.00779(2) 0.58217(2) 0.23115(2) 0.01750(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.378(8) . ?
C1 C4 1.498(8) . ?
C1 N1 1.359(7) . ?
C2 H2 0.9500 . ?
C2 C3 1.409(7) . ?
C3 C5 1.503(7) . ?
C3 N2 1.330(7) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.407(7) . ?
C6 C11 1.418(7) . ?
C6 N1 1.452(7) . ?
C7 C8 1.394(7) . ?
C7 C12 1.535(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.389(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.376(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.398(8) . ?
C11 C15 1.503(8) . ?
C12 H12 1.0000 . ?
C12 C13 1.547(7) . ?
C12 C14 1.523(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.567(8) . ?
C15 C17 1.538(8) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.412(7) . ?
C18 C23 1.392(7) . ?
C18 N2 1.466(6) . ?
C19 C20 1.398(7) . ?
C19 C24 1.527(8) . ?
C20 H20 0.9500 . ?
C20 C21 1.368(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.370(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.405(7) . ?
C23 C27 1.523(7) . ?
C24 H24 1.0000 . ?
C24 C25 1.524(9) . ?
C24 C26 1.503(9) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27 1.0000 . ?
C27 C28 1.544(7) . ?
C27 C29 1.515(8) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.418(7) . ?
C30 C35 1.423(7) . ?
C30 N3 1.429(6) . ?
C31 C32 1.412(7) . ?
C31 C36 1.501(8) . ?
C32 H32 0.9500 . ?
C32 C33 1.365(8) . ?
C33 H33 0.9500 . ?
C33 C34 1.387(8) . ?
C34 H34 0.9500 . ?
C34 C35 1.396(7) . ?
C35 C39 1.509(7) . ?
C36 H36 1.0000 . ?
C36 C37 1.559(7) . ?
C36 C38 1.530(8) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39 1.0000 . ?
C39 C40 1.539(7) . ?
C39 C41 1.522(7) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.519(7) . ?
C42 C44 1.534(7) . ?
C42 C45 1.545(7) . ?
C42 N4 1.495(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 N4 1.325(6) . ?
C46 O1 1.302(6) . ?
C46 O2 1.293(6) . ?
C46 Nb1 2.547(5) . ?
C47 C48 1.391(7) . ?
C47 C52 1.376(7) . ?
C47 B1 1.646(8) . ?
C48 C49 1.388(7) . ?
C48 F1 1.358(6) . ?
C49 C50 1.368(8) . ?
C49 F2 1.345(6) . ?
C50 C51 1.367(8) . ?
C50 F3 1.363(6) . ?
C51 C52 1.389(7) . ?
C51 F4 1.339(6) . ?
C52 F5 1.357(6) . ?
C53 C54 1.396(7) . ?
C53 C58 1.375(7) . ?
C53 B1 1.672(8) . ?
C54 C55 1.395(8) . ?
C54 F6 1.348(6) . ?
C55 C56 1.354(8) . ?
C55 F7 1.340(6) . ?
C56 C57 1.386(8) . ?
C56 F8 1.340(6) . ?
C57 C58 1.384(8) . ?
C57 F9 1.334(6) . ?
C58 F10 1.365(6) . ?
C59 C60 1.372(7) . ?
C59 C64 1.391(7) . ?
C59 B1 1.649(8) . ?
C60 C61 1.388(7) . ?
C60 F11 1.363(6) . ?
C61 C62 1.374(8) . ?
C61 F12 1.349(6) . ?
C62 C63 1.366(8) . ?
C62 F13 1.341(6) . ?
C63 C64 1.374(7) . ?
C63 F14 1.350(6) . ?
C64 F15 1.354(6) . ?
C65 C66 1.386(8) . ?
C65 C68 1.521(7) . ?
C65 N5 1.347(7) . ?
C66 H66 0.9500 . ?
C66 C67 1.379(7) . ?
C67 C69 1.520(7) . ?
C67 N6 1.342(7) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 C71 1.398(7) . ?
C70 C75 1.427(8) . ?
C70 N5 1.457(7) . ?
C71 C72 1.385(8) . ?
C71 C76 1.521(8) . ?
C72 H72 0.9500 . ?
C72 C73 1.371(8) . ?
C73 H73 0.9500 . ?
C73 C74 1.386(8) . ?
C74 H74 0.9500 . ?
C74 C75 1.404(8) . ?
C75 C79 1.538(8) . ?
C76 H76 1.0000 . ?
C76 C77 1.541(7) . ?
C76 C78 1.547(7) . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 H79 1.0000 . ?
C79 C80 1.525(10) . ?
C79 C81 1.540(9) . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 C83 1.404(7) . ?
C82 C87 1.411(7) . ?
C82 N6 1.462(6) . ?
C83 C84 1.394(7) . ?
C83 C88 1.515(7) . ?
C84 H84 0.9500 . ?
C84 C85 1.384(7) . ?
C85 H85 0.9500 . ?
C85 C86 1.385(8) . ?
C86 H86 0.9500 . ?
C86 C87 1.397(7) . ?
C87 C91 1.523(7) . ?
C88 H88 1.0000 . ?
C88 C89 1.538(7) . ?
C88 C90 1.532(7) . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
C91 H91 1.0000 . ?
C91 C92 1.533(8) . ?
C91 C93 1.521(8) . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?
C94 C95 1.419(8) . ?
C94 C99 1.414(8) . ?
C94 N7 1.430(6) . ?
C95 C96 1.383(8) . ?
C95 C100 1.510(8) . ?
C96 H96 0.9500 . ?
C96 C97 1.385(9) . ?
C97 H97 0.9500 . ?
C97 C98 1.372(10) . ?
C98 H98 0.9500 . ?
C98 C99 1.414(8) . ?
C99 C103 1.498(8) . ?
C100 H100 1.0000 . ?
C100 C101 1.521(8) . ?
C100 C102 1.548(8) . ?
C101 H10A 0.9800 . ?
C101 H10B 0.9800 . ?
C101 H10C 0.9800 . ?
C102 H10D 0.9800 . ?
C102 H10E 0.9800 . ?
C102 H10F 0.9800 . ?
C103 H103 1.0000 . ?
C103 C104 1.529(7) . ?
C103 C105 1.551(7) . ?
C104 H10G 0.9800 . ?
C104 H10H 0.9800 . ?
C104 H10I 0.9800 . ?
C105 H10J 0.9800 . ?
C105 H10K 0.9800 . ?
C105 H10L 0.9800 . ?
C106 C107 1.512(8) . ?
C106 C108 1.538(8) . ?
C106 C109 1.528(8) . ?
C106 N8 1.503(7) . ?
C107 H10M 0.9800 . ?
C107 H10N 0.9800 . ?
C107 H10O 0.9800 . ?
C108 H10P 0.9800 . ?
C108 H10Q 0.9800 . ?
C108 H10R 0.9800 . ?
C109 H10S 0.9800 . ?
C109 H10T 0.9800 . ?
C109 H10U 0.9800 . ?
C110 N8 1.327(6) . ?
C110 O3 1.315(6) . ?
C110 O4 1.284(6) . ?
C110 Nb2 2.564(5) . ?
C111 C112 1.387(7) . ?
C111 C116 1.389(7) . ?
C111 B2 1.653(8) . ?
C112 C113 1.400(8) . ?
C112 F16 1.357(6) . ?
C113 C114 1.355(8) . ?
C113 F17 1.343(6) . ?
C114 C115 1.381(8) . ?
C114 F18 1.353(6) . ?
C115 C116 1.374(8) . ?
C115 F19 1.345(6) . ?
C116 F20 1.354(6) . ?
C117 C118 1.399(8) . ?
C117 C122 1.390(7) . ?
C117 B2 1.642(8) . ?
C118 C119 1.369(8) . ?
C118 F21 1.353(6) . ?
C119 C120 1.382(9) . ?
C119 F22 1.362(7) . ?
C120 C121 1.370(9) . ?
C120 F23 1.350(7) . ?
C121 C122 1.383(8) . ?
C121 F24 1.335(7) . ?
C122 F25 1.353(6) . ?
C123 C124 1.379(7) . ?
C123 C128 1.400(7) . ?
C123 B2 1.618(8) . ?
C124 C125 1.407(8) . ?
C124 F26 1.338(6) . ?
C125 C126 1.340(8) . ?
C125 F27 1.365(6) . ?
C126 C127 1.400(8) . ?
C126 F28 1.349(6) . ?
C127 C128 1.376(7) . ?
C127 F29 1.331(6) . ?
C128 F30 1.360(6) . ?
C129 H12A 0.9800 . ?
C129 H12B 0.9800 . ?
C129 H12C 0.9800 . ?
C129 C130 1.484(11) . ?
C130 H13D 0.9900 . ?
C130 H13E 0.9900 . ?
C130 O5 1.479(9) . ?
C131 H13F 0.9900 . ?
C131 H13G 0.9900 . ?
C131 C132 1.455(11) . ?
C131 O5 1.433(9) . ?
C132 H13H 0.9800 . ?
C132 H13I 0.9800 . ?
C132 H13J 0.9800 . ?
C133 H13K 0.9800 . ?
C133 H13L 0.9800 . ?
C133 H13M 0.9800 . ?
C133 C134 1.504(14) . ?
C134 H13N 0.9900 . ?
C134 H13O 0.9900 . ?
C134 O6 1.474(12) . ?
C135 H13P 0.9900 . ?
C135 H13Q 0.9900 . ?
C135 C136 1.503(16) . ?
C135 O6 1.421(11) . ?
C136 H13R 0.9800 . ?
C136 H13S 0.9800 . ?
C136 H13T 0.9800 . ?
B1 O2 1.517(7) . ?
B2 O4 1.533(7) . ?
N1 Nb1 2.076(4) . ?
N2 Nb1 2.192(4) . ?
N3 Nb1 1.759(4) . ?
N4 Nb1 2.126(4) . ?
N5 Nb2 2.077(5) . ?
N6 Nb2 2.194(4) . ?
N7 Nb2 1.766(4) . ?
N8 Nb2 2.139(5) . ?
O1 Nb1 2.133(3) . ?
O3 Nb2 2.138(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C4 118.1(5) . . ?
N1 C1 C2 120.9(5) . . ?
N1 C1 C4 121.0(5) . . ?
C1 C2 H2 115.6 . . ?
C1 C2 C3 128.8(5) . . ?
C3 C2 H2 115.6 . . ?
C2 C3 C5 115.4(5) . . ?
N2 C3 C2 124.3(5) . . ?
N2 C3 C5 120.2(5) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 121.9(5) . . ?
C7 C6 N1 120.5(5) . . ?
C11 C6 N1 117.6(5) . . ?
C6 C7 C12 123.2(5) . . ?
C8 C7 C6 118.8(5) . . ?
C8 C7 C12 117.9(5) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 C7 119.9(5) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.8(5) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 119.0 . . ?
C9 C10 C11 122.1(5) . . ?
C11 C10 H10 119.0 . . ?
C6 C11 C15 122.2(5) . . ?
C10 C11 C6 116.5(5) . . ?
C10 C11 C15 121.2(5) . . ?
C7 C12 H12 107.8 . . ?
C7 C12 C13 111.0(4) . . ?
C13 C12 H12 107.8 . . ?
C14 C12 C7 112.8(5) . . ?
C14 C12 H12 107.8 . . ?
C14 C12 C13 109.4(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15 107.2 . . ?
C11 C15 C16 111.5(5) . . ?
C11 C15 C17 114.3(5) . . ?
C16 C15 H15 107.2 . . ?
C17 C15 H15 107.2 . . ?
C17 C15 C16 108.9(5) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N2 117.9(5) . . ?
C23 C18 C19 121.6(5) . . ?
C23 C18 N2 120.3(5) . . ?
C18 C19 C24 122.3(5) . . ?
C20 C19 C18 117.8(5) . . ?
C20 C19 C24 119.9(5) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 C19 120.8(5) . . ?
C21 C20 H20 119.6 . . ?
C20 C21 H21 119.5 . . ?
C20 C21 C22 121.0(5) . . ?
C22 C21 H21 119.5 . . ?
C21 C22 H22 119.6 . . ?
C21 C22 C23 120.9(5) . . ?
C23 C22 H22 119.6 . . ?
C18 C23 C22 117.8(5) . . ?
C18 C23 C27 121.8(5) . . ?
C22 C23 C27 120.3(5) . . ?
C19 C24 H24 108.4 . . ?
C25 C24 C19 112.7(5) . . ?
C25 C24 H24 108.4 . . ?
C26 C24 C19 110.7(5) . . ?
C26 C24 H24 108.4 . . ?
C26 C24 C25 108.2(5) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27 107.9 . . ?
C23 C27 C28 112.8(5) . . ?
C28 C27 H27 107.9 . . ?
C29 C27 C23 110.4(5) . . ?
C29 C27 H27 107.9 . . ?
C29 C27 C28 109.9(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C35 121.2(4) . . ?
C31 C30 N3 119.2(5) . . ?
C35 C30 N3 119.5(5) . . ?
C30 C31 C36 124.4(5) . . ?
C32 C31 C30 117.0(5) . . ?
C32 C31 C36 118.5(5) . . ?
C31 C32 H32 119.0 . . ?
C33 C32 C31 122.0(6) . . ?
C33 C32 H32 119.0 . . ?
C32 C33 H33 119.7 . . ?
C32 C33 C34 120.5(5) . . ?
C34 C33 H33 119.7 . . ?
C33 C34 H34 119.5 . . ?
C33 C34 C35 120.9(6) . . ?
C35 C34 H34 119.5 . . ?
C30 C35 C39 124.0(4) . . ?
C34 C35 C30 118.2(5) . . ?
C34 C35 C39 117.7(5) . . ?
C31 C36 H36 108.2 . . ?
C31 C36 C37 108.5(5) . . ?
C31 C36 C38 114.5(5) . . ?
C37 C36 H36 108.2 . . ?
C38 C36 H36 108.2 . . ?
C38 C36 C37 109.2(5) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C39 H39 107.6 . . ?
C35 C39 C40 111.8(4) . . ?
C35 C39 C41 111.8(4) . . ?
C40 C39 H39 107.6 . . ?
C41 C39 H39 107.6 . . ?
C41 C39 C40 110.3(5) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C44 109.1(4) . . ?
C43 C42 C45 109.0(4) . . ?
C44 C42 C45 110.9(5) . . ?
N4 C42 C43 107.2(4) . . ?
N4 C42 C44 112.2(4) . . ?
N4 C42 C45 108.2(4) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N4 C46 Nb1 56.5(3) . . ?
O1 C46 N4 113.3(5) . . ?
O1 C46 Nb1 56.8(3) . . ?
O2 C46 N4 122.9(5) . . ?
O2 C46 O1 123.8(5) . . ?
O2 C46 Nb1 178.1(4) . . ?
C48 C47 B1 118.0(5) . . ?
C52 C47 C48 114.5(5) . . ?
C52 C47 B1 127.3(5) . . ?
C49 C48 C47 123.7(5) . . ?
F1 C48 C47 119.7(5) . . ?
F1 C48 C49 116.5(5) . . ?
C50 C49 C48 118.5(5) . . ?
F2 C49 C48 120.7(5) . . ?
F2 C49 C50 120.8(5) . . ?
C51 C50 C49 120.7(5) . . ?
F3 C50 C49 119.3(5) . . ?
F3 C50 C51 120.0(5) . . ?
C50 C51 C52 118.8(5) . . ?
F4 C51 C50 119.7(5) . . ?
F4 C51 C52 121.5(5) . . ?
C47 C52 C51 123.7(5) . . ?
F5 C52 C47 122.0(5) . . ?
F5 C52 C51 114.2(5) . . ?
C54 C53 B1 118.8(5) . . ?
C58 C53 C54 113.6(5) . . ?
C58 C53 B1 126.9(5) . . ?
C55 C54 C53 123.5(5) . . ?
F6 C54 C53 120.4(5) . . ?
F6 C54 C55 116.1(5) . . ?
C56 C55 C54 119.7(5) . . ?
F7 C55 C54 120.4(5) . . ?
F7 C55 C56 119.9(5) . . ?
C55 C56 C57 119.5(5) . . ?
F8 C56 C55 120.5(5) . . ?
F8 C56 C57 120.0(5) . . ?
C58 C57 C56 118.7(5) . . ?
F9 C57 C56 120.4(5) . . ?
F9 C57 C58 120.9(5) . . ?
C53 C58 C57 124.8(5) . . ?
F10 C58 C53 120.9(5) . . ?
F10 C58 C57 114.2(5) . . ?
C60 C59 C64 113.8(5) . . ?
C60 C59 B1 126.1(5) . . ?
C64 C59 B1 119.6(5) . . ?
C59 C60 C61 124.2(5) . . ?
F11 C60 C59 120.8(5) . . ?
F11 C60 C61 115.0(5) . . ?
C62 C61 C60 119.1(5) . . ?
F12 C61 C60 120.4(5) . . ?
F12 C61 C62 120.4(5) . . ?
C63 C62 C61 119.0(5) . . ?
F13 C62 C61 120.7(5) . . ?
F13 C62 C63 120.3(5) . . ?
C62 C63 C64 119.9(5) . . ?
F14 C63 C62 120.2(5) . . ?
F14 C63 C64 119.8(5) . . ?
C63 C64 C59 123.8(5) . . ?
F15 C64 C59 119.2(5) . . ?
F15 C64 C63 117.0(5) . . ?
C66 C65 C68 118.0(5) . . ?
N5 C65 C66 122.1(5) . . ?
N5 C65 C68 119.8(5) . . ?
C65 C66 H66 115.9 . . ?
C67 C66 C65 128.2(6) . . ?
C67 C66 H66 115.9 . . ?
C66 C67 C69 114.7(5) . . ?
N6 C67 C66 125.1(5) . . ?
N6 C67 C69 120.2(5) . . ?
C65 C68 H68A 109.5 . . ?
C65 C68 H68B 109.5 . . ?
C65 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C67 C69 H69A 109.5 . . ?
C67 C69 H69B 109.5 . . ?
C67 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C71 C70 C75 121.9(5) . . ?
C71 C70 N5 119.8(5) . . ?
C75 C70 N5 118.3(5) . . ?
C70 C71 C76 123.7(5) . . ?
C72 C71 C70 117.7(5) . . ?
C72 C71 C76 118.6(5) . . ?
C71 C72 H72 118.8 . . ?
C73 C72 C71 122.3(6) . . ?
C73 C72 H72 118.8 . . ?
C72 C73 H73 120.0 . . ?
C72 C73 C74 120.0(6) . . ?
C74 C73 H73 120.0 . . ?
C73 C74 H74 119.5 . . ?
C73 C74 C75 121.0(6) . . ?
C75 C74 H74 119.5 . . ?
C70 C75 C79 121.9(5) . . ?
C74 C75 C70 117.1(5) . . ?
C74 C75 C79 120.9(6) . . ?
C71 C76 H76 108.2 . . ?
C71 C76 C77 111.3(5) . . ?
C71 C76 C78 111.4(5) . . ?
C77 C76 H76 108.2 . . ?
C77 C76 C78 109.5(4) . . ?
C78 C76 H76 108.2 . . ?
C76 C77 H77A 109.5 . . ?
C76 C77 H77B 109.5 . . ?
C76 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C76 C78 H78A 109.5 . . ?
C76 C78 H78B 109.5 . . ?
C76 C78 H78C 109.5 . . ?
H78A C78 H78B 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C75 C79 H79 107.4 . . ?
C75 C79 C81 113.5(6) . . ?
C80 C79 C75 110.8(5) . . ?
C80 C79 H79 107.4 . . ?
C80 C79 C81 110.0(5) . . ?
C81 C79 H79 107.4 . . ?
C79 C80 H80A 109.5 . . ?
C79 C80 H80B 109.5 . . ?
C79 C80 H80C 109.5 . . ?
H80A C80 H80B 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C79 C81 H81A 109.5 . . ?
C79 C81 H81B 109.5 . . ?
C79 C81 H81C 109.5 . . ?
H81A C81 H81B 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C83 C82 C87 122.4(5) . . ?
C83 C82 N6 119.3(4) . . ?
C87 C82 N6 117.8(4) . . ?
C82 C83 C88 122.2(5) . . ?
C84 C83 C82 117.5(5) . . ?
C84 C83 C88 120.3(5) . . ?
C83 C84 H84 119.1 . . ?
C85 C84 C83 121.8(5) . . ?
C85 C84 H84 119.1 . . ?
C84 C85 H85 120.5 . . ?
C84 C85 C86 119.0(5) . . ?
C86 C85 H85 120.5 . . ?
C85 C86 H86 118.7 . . ?
C85 C86 C87 122.5(5) . . ?
C87 C86 H86 118.7 . . ?
C82 C87 C91 122.6(5) . . ?
C86 C87 C82 116.5(5) . . ?
C86 C87 C91 120.9(5) . . ?
C83 C88 H88 107.7 . . ?
C83 C88 C89 113.5(4) . . ?
C83 C88 C90 110.6(5) . . ?
C89 C88 H88 107.7 . . ?
C90 C88 H88 107.7 . . ?
C90 C88 C89 109.5(4) . . ?
C88 C89 H89A 109.5 . . ?
C88 C89 H89B 109.5 . . ?
C88 C89 H89C 109.5 . . ?
H89A C89 H89B 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
C88 C90 H90A 109.5 . . ?
C88 C90 H90B 109.5 . . ?
C88 C90 H90C 109.5 . . ?
H90A C90 H90B 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
C87 C91 H91 107.4 . . ?
C87 C91 C92 111.2(5) . . ?
C92 C91 H91 107.4 . . ?
C93 C91 C87 112.8(5) . . ?
C93 C91 H91 107.4 . . ?
C93 C91 C92 110.4(5) . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92B 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
C91 C93 H93A 109.5 . . ?
C91 C93 H93B 109.5 . . ?
C91 C93 H93C 109.5 . . ?
H93A C93 H93B 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
C95 C94 N7 119.9(5) . . ?
C99 C94 C95 121.0(5) . . ?
C99 C94 N7 119.0(5) . . ?
C94 C95 C100 123.1(5) . . ?
C96 C95 C94 117.9(6) . . ?
C96 C95 C100 119.0(6) . . ?
C95 C96 H96 118.8 . . ?
C95 C96 C97 122.5(6) . . ?
C97 C96 H96 118.8 . . ?
C96 C97 H97 120.4 . . ?
C98 C97 C96 119.1(6) . . ?
C98 C97 H97 120.4 . . ?
C97 C98 H98 119.0 . . ?
C97 C98 C99 122.1(6) . . ?
C99 C98 H98 119.0 . . ?
C94 C99 C103 123.3(5) . . ?
C98 C99 C94 117.2(6) . . ?
C98 C99 C103 119.4(5) . . ?
C95 C100 H100 108.3 . . ?
C95 C100 C101 112.4(5) . . ?
C95 C100 C102 110.7(5) . . ?
C101 C100 H100 108.3 . . ?
C101 C100 C102 108.7(5) . . ?
C102 C100 H100 108.3 . . ?
C100 C101 H10A 109.5 . . ?
C100 C101 H10B 109.5 . . ?
C100 C101 H10C 109.5 . . ?
H10A C101 H10B 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
C100 C102 H10D 109.5 . . ?
C100 C102 H10E 109.5 . . ?
C100 C102 H10F 109.5 . . ?
H10D C102 H10E 109.5 . . ?
H10D C102 H10F 109.5 . . ?
H10E C102 H10F 109.5 . . ?
C99 C103 H103 108.3 . . ?
C99 C103 C104 109.6(5) . . ?
C99 C103 C105 114.1(5) . . ?
C104 C103 H103 108.3 . . ?
C104 C103 C105 107.9(5) . . ?
C105 C103 H103 108.3 . . ?
C103 C104 H10G 109.5 . . ?
C103 C104 H10H 109.5 . . ?
C103 C104 H10I 109.5 . . ?
H10G C104 H10H 109.5 . . ?
H10G C104 H10I 109.5 . . ?
H10H C104 H10I 109.5 . . ?
C103 C105 H10J 109.5 . . ?
C103 C105 H10K 109.5 . . ?
C103 C105 H10L 109.5 . . ?
H10J C105 H10K 109.5 . . ?
H10J C105 H10L 109.5 . . ?
H10K C105 H10L 109.5 . . ?
C107 C106 C108 111.7(5) . . ?
C107 C106 C109 109.0(5) . . ?
C109 C106 C108 109.9(5) . . ?
N8 C106 C107 108.9(5) . . ?
N8 C106 C108 110.6(4) . . ?
N8 C106 C109 106.5(5) . . ?
C106 C107 H10M 109.5 . . ?
C106 C107 H10N 109.5 . . ?
C106 C107 H10O 109.5 . . ?
H10M C107 H10N 109.5 . . ?
H10M C107 H10O 109.5 . . ?
H10N C107 H10O 109.5 . . ?
C106 C108 H10P 109.5 . . ?
C106 C108 H10Q 109.5 . . ?
C106 C108 H10R 109.5 . . ?
H10P C108 H10Q 109.5 . . ?
H10P C108 H10R 109.5 . . ?
H10Q C108 H10R 109.5 . . ?
C106 C109 H10S 109.5 . . ?
C106 C109 H10T 109.5 . . ?
C106 C109 H10U 109.5 . . ?
H10S C109 H10T 109.5 . . ?
H10S C109 H10U 109.5 . . ?
H10T C109 H10U 109.5 . . ?
N8 C110 Nb2 56.4(3) . . ?
O3 C110 N8 112.8(5) . . ?
O3 C110 Nb2 56.4(3) . . ?
O4 C110 N8 123.3(5) . . ?
O4 C110 O3 123.8(5) . . ?
O4 C110 Nb2 179.3(4) . . ?
C112 C111 C116 113.4(5) . . ?
C112 C111 B2 127.3(5) . . ?
C116 C111 B2 119.0(5) . . ?
C111 C112 C113 123.7(5) . . ?
F16 C112 C111 121.5(5) . . ?
F16 C112 C113 114.8(5) . . ?
C114 C113 C112 119.3(5) . . ?
F17 C113 C112 120.1(5) . . ?
F17 C113 C114 120.6(5) . . ?
C113 C114 C115 119.9(5) . . ?
F18 C114 C113 120.9(5) . . ?
F18 C114 C115 119.1(5) . . ?
C116 C115 C114 118.7(5) . . ?
F19 C115 C114 119.8(5) . . ?
F19 C115 C116 121.4(5) . . ?
C115 C116 C111 124.8(5) . . ?
F20 C116 C111 120.1(5) . . ?
F20 C116 C115 115.0(5) . . ?
C118 C117 B2 118.9(5) . . ?
C122 C117 C118 113.5(5) . . ?
C122 C117 B2 126.9(5) . . ?
C119 C118 C117 124.3(5) . . ?
F21 C118 C117 119.2(5) . . ?
F21 C118 C119 116.5(5) . . ?
C118 C119 C120 119.4(6) . . ?
F22 C119 C118 121.1(5) . . ?
F22 C119 C120 119.4(5) . . ?
C121 C120 C119 119.3(6) . . ?
F23 C120 C119 119.7(6) . . ?
F23 C120 C121 121.0(6) . . ?
C120 C121 C122 119.5(6) . . ?
F24 C121 C120 120.4(6) . . ?
F24 C121 C122 120.1(6) . . ?
C121 C122 C117 124.0(6) . . ?
F25 C122 C117 119.7(5) . . ?
F25 C122 C121 116.3(5) . . ?
C124 C123 C128 113.9(5) . . ?
C124 C123 B2 126.9(5) . . ?
C128 C123 B2 119.1(5) . . ?
C123 C124 C125 122.5(5) . . ?
F26 C124 C123 121.6(5) . . ?
F26 C124 C125 115.9(5) . . ?
C126 C125 C124 120.7(5) . . ?
C126 C125 F27 120.0(5) . . ?
F27 C125 C124 119.3(5) . . ?
C125 C126 C127 119.9(5) . . ?
C125 C126 F28 120.7(5) . . ?
F28 C126 C127 119.3(5) . . ?
C128 C127 C126 117.5(5) . . ?
F29 C127 C126 120.5(5) . . ?
F29 C127 C128 122.0(5) . . ?
C127 C128 C123 125.4(5) . . ?
F30 C128 C123 119.1(4) . . ?
F30 C128 C127 115.5(5) . . ?
H12A C129 H12B 109.5 . . ?
H12A C129 H12C 109.5 . . ?
H12B C129 H12C 109.5 . . ?
C130 C129 H12A 109.5 . . ?
C130 C129 H12B 109.5 . . ?
C130 C129 H12C 109.5 . . ?
C129 C130 H13D 110.3 . . ?
C129 C130 H13E 110.3 . . ?
H13D C130 H13E 108.6 . . ?
O5 C130 C129 106.9(7) . . ?
O5 C130 H13D 110.3 . . ?
O5 C130 H13E 110.3 . . ?
H13F C131 H13G 108.3 . . ?
C132 C131 H13F 109.9 . . ?
C132 C131 H13G 109.9 . . ?
O5 C131 H13F 109.9 . . ?
O5 C131 H13G 109.9 . . ?
O5 C131 C132 108.9(7) . . ?
C131 C132 H13H 109.5 . . ?
C131 C132 H13I 109.5 . . ?
C131 C132 H13J 109.5 . . ?
H13H C132 H13I 109.5 . . ?
H13H C132 H13J 109.5 . . ?
H13I C132 H13J 109.5 . . ?
H13K C133 H13L 109.5 . . ?
H13K C133 H13M 109.5 . . ?
H13L C133 H13M 109.5 . . ?
C134 C133 H13K 109.5 . . ?
C134 C133 H13L 109.5 . . ?
C134 C133 H13M 109.5 . . ?
C133 C134 H13N 108.9 . . ?
C133 C134 H13O 108.9 . . ?
H13N C134 H13O 107.7 . . ?
O6 C134 C133 113.3(10) . . ?
O6 C134 H13N 108.9 . . ?
O6 C134 H13O 108.9 . . ?
H13P C135 H13Q 107.1 . . ?
C136 C135 H13P 107.6 . . ?
C136 C135 H13Q 107.6 . . ?
O6 C135 H13P 107.6 . . ?
O6 C135 H13Q 107.6 . . ?
O6 C135 C136 118.7(11) . . ?
C135 C136 H13R 109.5 . . ?
C135 C136 H13S 109.5 . . ?
C135 C136 H13T 109.5 . . ?
H13R C136 H13S 109.5 . . ?
H13R C136 H13T 109.5 . . ?
H13S C136 H13T 109.5 . . ?
C47 B1 C53 111.3(4) . . ?
C47 B1 C59 115.6(4) . . ?
C59 B1 C53 104.3(4) . . ?
O2 B1 C47 109.3(4) . . ?
O2 B1 C53 104.5(4) . . ?
O2 B1 C59 111.2(4) . . ?
C117 B2 C111 102.9(5) . . ?
C123 B2 C111 112.8(4) . . ?
C123 B2 C117 116.8(5) . . ?
O4 B2 C111 101.8(4) . . ?
O4 B2 C117 111.4(4) . . ?
O4 B2 C123 109.9(5) . . ?
C1 N1 C6 120.0(4) . . ?
C1 N1 Nb1 129.7(4) . . ?
C6 N1 Nb1 109.7(3) . . ?
C3 N2 C18 113.1(4) . . ?
C3 N2 Nb1 123.5(4) . . ?
C18 N2 Nb1 123.1(3) . . ?
C30 N3 Nb1 174.0(4) . . ?
C42 N4 Nb1 144.3(3) . . ?
C46 N4 C42 123.4(4) . . ?
C46 N4 Nb1 92.2(3) . . ?
C65 N5 C70 120.7(5) . . ?
C65 N5 Nb2 129.6(4) . . ?
C70 N5 Nb2 109.1(4) . . ?
C67 N6 C82 113.3(4) . . ?
C67 N6 Nb2 123.6(4) . . ?
C82 N6 Nb2 123.1(3) . . ?
C94 N7 Nb2 171.1(4) . . ?
C106 N8 Nb2 143.8(4) . . ?
C110 N8 C106 123.6(5) . . ?
C110 N8 Nb2 92.4(3) . . ?
C46 O1 Nb1 92.5(3) . . ?
C46 O2 B1 132.1(4) . . ?
C110 O3 Nb2 92.8(3) . . ?
C110 O4 B2 132.0(4) . . ?
C131 O5 C130 112.0(6) . . ?
C135 O6 C134 121.6(10) . . ?
N1 Nb1 C46 133.62(16) . . ?
N1 Nb1 N2 83.80(16) . . ?
N1 Nb1 N4 118.27(16) . . ?
N1 Nb1 O1 134.70(14) . . ?
N2 Nb1 C46 109.63(16) . . ?
N3 Nb1 C46 116.81(18) . . ?
N3 Nb1 N1 103.74(18) . . ?
N3 Nb1 N2 98.94(17) . . ?
N3 Nb1 N4 105.86(18) . . ?
N3 Nb1 O1 120.14(16) . . ?
N4 Nb1 C46 31.33(15) . . ?
N4 Nb1 N2 140.58(16) . . ?
N4 Nb1 O1 62.04(14) . . ?
O1 Nb1 C46 30.72(14) . . ?
O1 Nb1 N2 79.11(14) . . ?
N5 Nb2 C110 133.13(17) . . ?
N5 Nb2 N6 84.03(17) . . ?
N5 Nb2 N8 119.13(17) . . ?
N5 Nb2 O3 133.87(15) . . ?
N6 Nb2 C110 108.98(16) . . ?
N7 Nb2 C110 117.54(18) . . ?
N7 Nb2 N5 103.84(19) . . ?
N7 Nb2 N6 98.65(18) . . ?
N7 Nb2 N8 105.73(18) . . ?
N7 Nb2 O3 120.69(17) . . ?
N8 Nb2 C110 31.13(16) . . ?
N8 Nb2 N6 139.93(16) . . ?
O3 Nb2 C110 30.82(14) . . ?
O3 Nb2 N6 78.34(15) . . ?
O3 Nb2 N8 61.95(15) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Diethyl ether'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bmkxr68
_database_code_depnum_ccdc_archive 'CCDC 2004135'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-14 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_bmkxr68             
;
PROBLEM: Check Calcd Positive Resid. Density on       Nb1       1.62 eA-3  
RESPONSE: Possible minor unresolved twinning or disorder at a heavy atom.
;
# end Validation Reply Form
_audit_creation_date             2020-05-13
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            '[(BDI)Nb(NAr)(μ-CO3)]2'
_chemical_name_systematic        
'bis(μ2-carbonato-O,O?:O??)-bis(2,6-diisopropylphenyl)imino-bis(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-diniobium(V) hexamethydisiloxane solvate'
_chemical_formula_moiety         'C84 H116 N6 Nb2 O6, 2(C6 H18 O Si2)'
_chemical_formula_sum            'C96 H152 N6 Nb2 O8 Si4'
_chemical_formula_weight         908.20
_chemical_melting_point          444
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.3294(12)
_cell_length_b                   15.6578(14)
_cell_length_c                   24.934(2)
_cell_angle_alpha                76.581(4)
_cell_angle_beta                 81.666(4)
_cell_angle_gamma                83.559(4)
_cell_volume                     4991.7(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9087
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      2.25
_shelx_estimated_absorpt_T_max   0.968
_shelx_estimated_absorpt_T_min   0.955
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1279 before and 0.0678 after correction.
The Ratio of minimum to maximum transmission is 0.8968.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1465
_diffrn_reflns_av_unetI/netI     0.0994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            85465
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.341
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12832
_reflns_number_total             18437
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.737
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1079
_refine_ls_number_reflns         18437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0603
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0950P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1698
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C42) = Uanis(O3)
3.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C36(H36), C39(H39), C54(H54),
 C57(H57), C66(H66), C69(H69), C78(H78), C81(H81)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32),
 C33(H33), C34(H34), C44(H44), C50(H50), C51(H51), C52(H52), C62(H62), C63(H63),
  C64(H64), C74(H74), C75(H75), C76(H76)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,
 H70B,H70C), C71(H71A,H71B,H71C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C),
 C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C85(H85A,H85B,H85C), C86(H86A,H86B,
 H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,
 H90B,H90C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C),
 C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6475(3) 1.2193(3) 0.68528(15) 0.0243(9) Uani 1 1 d . . . . .
C2 C 0.7067(3) 1.2369(3) 0.72319(16) 0.0255(9) Uani 1 1 d . . . . .
H2 H 0.728338 1.294784 0.714938 0.031 Uiso 1 1 calc R . . . .
C3 C 0.7383(3) 1.1812(3) 0.77129(15) 0.0258(9) Uani 1 1 d . . . . .
C4 C 0.6122(3) 1.2977(3) 0.64401(16) 0.0295(9) Uani 1 1 d . . . . .
H4A H 0.656890 1.301789 0.608807 0.044 Uiso 1 1 calc GR . . . .
H4B H 0.613985 1.350959 0.658010 0.044 Uiso 1 1 calc GR . . . .
H4C H 0.542418 1.291954 0.638025 0.044 Uiso 1 1 calc GR . . . .
C5 C 0.7851(3) 1.2245(3) 0.80861(16) 0.0345(10) Uani 1 1 d . . . . .
H5A H 0.769433 1.193231 0.847337 0.052 Uiso 1 1 calc GR . . . .
H5B H 0.757262 1.285992 0.804313 0.052 Uiso 1 1 calc GR . . . .
H5C H 0.859016 1.222339 0.798464 0.052 Uiso 1 1 calc GR . . . .
C6 C 0.5490(3) 1.1329(3) 0.64965(15) 0.0229(9) Uani 1 1 d . . . . .
C7 C 0.5824(3) 1.1276(3) 0.59426(15) 0.0255(9) Uani 1 1 d . . . . .
C8 C 0.5091(3) 1.1183(3) 0.56122(15) 0.0312(10) Uani 1 1 d . . . . .
H8 H 0.530006 1.113788 0.523834 0.037 Uiso 1 1 calc R . . . .
C9 C 0.4088(3) 1.1157(3) 0.58170(16) 0.0357(11) Uani 1 1 d . . . . .
H9 H 0.360835 1.108474 0.558718 0.043 Uiso 1 1 calc R . . . .
C10 C 0.3760(3) 1.1236(3) 0.63601(16) 0.0326(10) Uani 1 1 d . . . . .
H10 H 0.305649 1.122679 0.649532 0.039 Uiso 1 1 calc R . . . .
C11 C 0.4448(3) 1.1329(3) 0.67081(15) 0.0257(9) Uani 1 1 d . . . . .
C12 C 0.6931(3) 1.1304(3) 0.56935(15) 0.0284(10) Uani 1 1 d . . . . .
H12 H 0.732763 1.141792 0.597723 0.034 Uiso 1 1 calc R . . . .
C13 C 0.7077(3) 1.2052(3) 0.51736(16) 0.0415(12) Uani 1 1 d . . . . .
H13A H 0.675627 1.192323 0.487487 0.062 Uiso 1 1 calc GR . . . .
H13B H 0.780551 1.210252 0.505383 0.062 Uiso 1 1 calc GR . . . .
H13C H 0.676265 1.260853 0.526079 0.062 Uiso 1 1 calc GR . . . .
C14 C 0.7353(3) 1.0426(3) 0.55558(16) 0.0373(11) Uani 1 1 d . . . . .
H14A H 0.723320 0.995208 0.588628 0.056 Uiso 1 1 calc GR . . . .
H14B H 0.808577 1.043893 0.543581 0.056 Uiso 1 1 calc GR . . . .
H14C H 0.701267 1.032225 0.525654 0.056 Uiso 1 1 calc GR . . . .
C15 C 0.4037(3) 1.1468(3) 0.72822(16) 0.0324(10) Uani 1 1 d . . . . .
H15 H 0.462482 1.139298 0.750121 0.039 Uiso 1 1 calc R . . . .
C16 C 0.3543(4) 1.2413(3) 0.7249(2) 0.0514(13) Uani 1 1 d . . . . .
H16A H 0.403283 1.283407 0.704860 0.077 Uiso 1 1 calc GR . . . .
H16B H 0.334083 1.250985 0.762583 0.077 Uiso 1 1 calc GR . . . .
H16C H 0.294188 1.249568 0.705297 0.077 Uiso 1 1 calc GR . . . .
C17 C 0.3280(3) 1.0812(3) 0.75954(17) 0.0417(12) Uani 1 1 d . . . . .
H17A H 0.269412 1.087039 0.738915 0.063 Uiso 1 1 calc GR . . . .
H17B H 0.304969 1.092939 0.796469 0.063 Uiso 1 1 calc GR . . . .
H17C H 0.360807 1.021192 0.763384 0.063 Uiso 1 1 calc GR . . . .
C18 C 0.7323(3) 1.0504(3) 0.84243(14) 0.0226(9) Uani 1 1 d . . . . .
C19 C 0.6452(3) 1.0564(3) 0.88044(15) 0.0264(9) Uani 1 1 d . . . . .
C20 C 0.6513(3) 1.0176(3) 0.93559(16) 0.0370(11) Uani 1 1 d . . . . .
H20 H 0.592915 1.021870 0.961960 0.044 Uiso 1 1 calc R . . . .
C21 C 0.7397(3) 0.9728(3) 0.95366(17) 0.0408(12) Uani 1 1 d . . . . .
H21 H 0.742207 0.946565 0.991874 0.049 Uiso 1 1 calc R . . . .
C22 C 0.8241(3) 0.9668(3) 0.91529(16) 0.0376(11) Uani 1 1 d . . . . .
H22 H 0.884112 0.933869 0.927397 0.045 Uiso 1 1 calc R . . . .
C23 C 0.8242(3) 1.0071(3) 0.85951(16) 0.0298(10) Uani 1 1 d . . . . .
C24 C 0.5461(3) 1.1053(3) 0.86189(16) 0.0340(11) Uani 1 1 d . . . . .
H24 H 0.552292 1.115463 0.820481 0.041 Uiso 1 1 calc R . . . .
C25 C 0.4551(3) 1.0529(3) 0.88545(18) 0.0458(13) Uani 1 1 d . . . . .
H25A H 0.465458 0.996405 0.873988 0.069 Uiso 1 1 calc GR . . . .
H25B H 0.393790 1.086004 0.871553 0.069 Uiso 1 1 calc GR . . . .
H25C H 0.446982 1.042130 0.926100 0.069 Uiso 1 1 calc GR . . . .
C26 C 0.5291(4) 1.1959(3) 0.8773(2) 0.0534(14) Uani 1 1 d . . . . .
H26A H 0.467063 1.227407 0.863319 0.080 Uiso 1 1 calc GR . . . .
H26B H 0.587367 1.230157 0.860662 0.080 Uiso 1 1 calc GR . . . .
H26C H 0.521942 1.187893 0.917821 0.080 Uiso 1 1 calc GR . . . .
C27 C 0.9223(3) 1.0021(3) 0.82047(17) 0.0418(12) Uani 1 1 d . . . . .
H27 H 0.906882 1.031435 0.782100 0.050 Uiso 1 1 calc R . . . .
C28 C 0.9646(3) 0.9087(4) 0.8195(2) 0.0516(14) Uani 1 1 d . . . . .
H28A H 0.986918 0.880054 0.855588 0.077 Uiso 1 1 calc GR . . . .
H28B H 1.022526 0.909458 0.790347 0.077 Uiso 1 1 calc GR . . . .
H28C H 0.911636 0.875985 0.811899 0.077 Uiso 1 1 calc GR . . . .
C29 C 1.0029(3) 1.0533(3) 0.8351(2) 0.0492(13) Uani 1 1 d . . . . .
H29A H 0.975518 1.114273 0.834426 0.074 Uiso 1 1 calc GR . . . .
H29B H 1.063853 1.052956 0.807897 0.074 Uiso 1 1 calc GR . . . .
H29C H 1.020777 1.025336 0.872295 0.074 Uiso 1 1 calc GR . . . .
C30 C 0.9197(3) 1.0403(3) 0.64460(16) 0.0281(9) Uani 1 1 d . . . . .
C31 C 0.9720(3) 1.1177(3) 0.63039(19) 0.0406(11) Uani 1 1 d . . . . .
C32 C 1.0617(3) 1.1176(3) 0.5940(2) 0.0504(14) Uani 1 1 d . . . . .
H32 H 1.097048 1.169447 0.583240 0.060 Uiso 1 1 calc R . . . .
C33 C 1.1002(4) 1.0469(4) 0.5733(2) 0.0549(15) Uani 1 1 d . . . . .
H33 H 1.161838 1.049322 0.548727 0.066 Uiso 1 1 calc R . . . .
C34 C 1.0499(3) 0.9708(3) 0.5881(2) 0.0487(13) Uani 1 1 d . . . . .
H34 H 1.078220 0.921065 0.573740 0.058 Uiso 1 1 calc R . . . .
C35 C 0.9592(3) 0.9653(3) 0.62332(17) 0.0310(10) Uani 1 1 d . . . . .
C36 C 0.9334(4) 1.1980(3) 0.6528(2) 0.0585(16) Uani 1 1 d . . . . .
H36 H 0.867851 1.184830 0.676983 0.070 Uiso 1 1 calc R . . . .
C37 C 0.9113(4) 1.2782(4) 0.6074(3) 0.0708(18) Uani 1 1 d . . . . .
H37A H 0.975382 1.297692 0.585883 0.106 Uiso 1 1 calc GR . . . .
H37B H 0.875927 1.325775 0.624211 0.106 Uiso 1 1 calc GR . . . .
H37C H 0.868303 1.263051 0.582854 0.106 Uiso 1 1 calc GR . . . .
C38 C 1.0062(5) 1.2174(4) 0.6889(2) 0.078(2) Uani 1 1 d . . . . .
H38A H 1.069863 1.234634 0.665854 0.118 Uiso 1 1 calc GR . . . .
H38B H 1.020305 1.164543 0.717540 0.118 Uiso 1 1 calc GR . . . .
H38C H 0.975637 1.265447 0.706536 0.118 Uiso 1 1 calc GR . . . .
C39 C 0.9090(3) 0.8802(3) 0.63997(16) 0.0303(10) Uani 1 1 d . . . . .
H39 H 0.835456 0.893970 0.652380 0.036 Uiso 1 1 calc R . . . .
C40 C 0.9158(3) 0.8345(3) 0.59101(17) 0.0356(10) Uani 1 1 d . . . . .
H40A H 0.890790 0.876333 0.559061 0.053 Uiso 1 1 calc GR . . . .
H40B H 0.874145 0.784086 0.601830 0.053 Uiso 1 1 calc GR . . . .
H40C H 0.986738 0.814028 0.580971 0.053 Uiso 1 1 calc GR . . . .
C41 C 0.9554(3) 0.8175(3) 0.68878(17) 0.0379(11) Uani 1 1 d . . . . .
H41A H 1.027897 0.803601 0.677750 0.057 Uiso 1 1 calc GR . . . .
H41B H 0.920563 0.763045 0.699255 0.057 Uiso 1 1 calc GR . . . .
H41C H 0.947322 0.845723 0.720516 0.057 Uiso 1 1 calc GR . . . .
C42 C 0.5601(3) 0.9313(2) 0.73541(15) 0.0210(5) Uani 1 1 d . . . . .
C43 C 0.4312(3) 0.6140(3) 0.87040(15) 0.0307(10) Uani 1 1 d . . . . .
C44 C 0.5025(3) 0.5426(3) 0.86752(15) 0.0306(10) Uani 1 1 d . . . . .
H44 H 0.477621 0.486027 0.880794 0.037 Uiso 1 1 calc R . . . .
C45 C 0.6072(3) 0.5434(3) 0.84741(15) 0.0297(10) Uani 1 1 d . . . . .
C46 C 0.3307(3) 0.5938(3) 0.90521(18) 0.0394(11) Uani 1 1 d . . . . .
H46A H 0.310973 0.637302 0.928236 0.059 Uiso 1 1 calc GR . . . .
H46B H 0.337325 0.534743 0.929176 0.059 Uiso 1 1 calc GR . . . .
H46C H 0.278556 0.596259 0.880812 0.059 Uiso 1 1 calc GR . . . .
C47 C 0.6663(3) 0.4556(3) 0.85851(18) 0.0402(11) Uani 1 1 d . . . . .
H47A H 0.673840 0.430526 0.825458 0.060 Uiso 1 1 calc GR . . . .
H47B H 0.630212 0.416062 0.889900 0.060 Uiso 1 1 calc GR . . . .
H47C H 0.733754 0.462577 0.867434 0.060 Uiso 1 1 calc GR . . . .
C48 C 0.3811(3) 0.7686(3) 0.86216(15) 0.0276(9) Uani 1 1 d . . . . .
C49 C 0.3962(3) 0.7941(3) 0.91046(16) 0.0307(10) Uani 1 1 d . . . . .
C50 C 0.3300(3) 0.8614(3) 0.92666(18) 0.0370(11) Uani 1 1 d . . . . .
H50 H 0.336697 0.878297 0.960104 0.044 Uiso 1 1 calc R . . . .
C51 C 0.2559(3) 0.9035(3) 0.89539(18) 0.0371(11) Uani 1 1 d . . . . .
H51 H 0.213491 0.951064 0.906279 0.045 Uiso 1 1 calc R . . . .
C52 C 0.2422(3) 0.8773(3) 0.84803(18) 0.0377(11) Uani 1 1 d . . . . .
H52 H 0.189289 0.906448 0.827056 0.045 Uiso 1 1 calc R . . . .
C53 C 0.3037(3) 0.8096(3) 0.83044(17) 0.0324(10) Uani 1 1 d . . . . .
C54 C 0.4796(3) 0.7508(3) 0.94538(17) 0.0409(12) Uani 1 1 d . . . . .
H54 H 0.523730 0.710067 0.924696 0.049 Uiso 1 1 calc R . . . .
C55 C 0.5459(3) 0.8183(4) 0.95343(18) 0.0476(13) Uani 1 1 d . . . . .
H55A H 0.574705 0.851194 0.917093 0.071 Uiso 1 1 calc GR . . . .
H55B H 0.601091 0.788241 0.974557 0.071 Uiso 1 1 calc GR . . . .
H55C H 0.504711 0.859156 0.973839 0.071 Uiso 1 1 calc GR . . . .
C56 C 0.4375(5) 0.6955(4) 1.00190(19) 0.0624(16) Uani 1 1 d . . . . .
H56A H 0.493996 0.669169 1.023099 0.094 Uiso 1 1 calc GR . . . .
H56B H 0.400090 0.648694 0.996017 0.094 Uiso 1 1 calc GR . . . .
H56C H 0.391674 0.733321 1.022613 0.094 Uiso 1 1 calc GR . . . .
C57 C 0.2820(3) 0.7804(3) 0.77960(19) 0.0438(12) Uani 1 1 d . . . . .
H57 H 0.341265 0.740538 0.768239 0.053 Uiso 1 1 calc R . . . .
C58 C 0.2679(4) 0.8584(4) 0.73066(18) 0.0570(15) Uani 1 1 d . . . . .
H58A H 0.203490 0.892750 0.738542 0.086 Uiso 1 1 calc GR . . . .
H58B H 0.266758 0.836617 0.696975 0.086 Uiso 1 1 calc GR . . . .
H58C H 0.324289 0.895913 0.725126 0.086 Uiso 1 1 calc GR . . . .
C59 C 0.1867(4) 0.7291(3) 0.7927(2) 0.0539(14) Uani 1 1 d . . . . .
H59A H 0.195781 0.678157 0.823398 0.081 Uiso 1 1 calc GR . . . .
H59B H 0.175929 0.708899 0.759722 0.081 Uiso 1 1 calc GR . . . .
H59C H 0.127516 0.767557 0.803191 0.081 Uiso 1 1 calc GR . . . .
C60 C 0.7616(3) 0.6081(3) 0.81372(16) 0.0276(9) Uani 1 1 d . . . . .
C61 C 0.8141(3) 0.5826(3) 0.76611(17) 0.0326(10) Uani 1 1 d . . . . .
C62 C 0.9192(3) 0.5772(3) 0.75915(19) 0.0374(11) Uani 1 1 d . . . . .
H62 H 0.955995 0.560804 0.727003 0.045 Uiso 1 1 calc R . . . .
C63 C 0.9708(4) 0.5956(3) 0.7987(2) 0.0486(13) Uani 1 1 d . . . . .
H63 H 1.043059 0.591192 0.793755 0.058 Uiso 1 1 calc R . . . .
C64 C 0.9186(3) 0.6202(3) 0.84542(19) 0.0406(11) Uani 1 1 d . . . . .
H64 H 0.955455 0.632334 0.872304 0.049 Uiso 1 1 calc R . . . .
C65 C 0.8139(3) 0.6274(3) 0.85368(17) 0.0331(10) Uani 1 1 d . . . . .
C66 C 0.7601(3) 0.5608(3) 0.72155(17) 0.0331(10) Uani 1 1 d . . . . .
H66 H 0.685695 0.561170 0.735039 0.040 Uiso 1 1 calc R . . . .
C67 C 0.7746(3) 0.6306(3) 0.66750(17) 0.0368(11) Uani 1 1 d . . . . .
H67A H 0.751221 0.688889 0.674860 0.055 Uiso 1 1 calc GR . . . .
H67B H 0.734984 0.618127 0.640422 0.055 Uiso 1 1 calc GR . . . .
H67C H 0.846772 0.629612 0.652586 0.055 Uiso 1 1 calc GR . . . .
C68 C 0.7964(4) 0.4698(3) 0.71018(19) 0.0454(12) Uani 1 1 d . . . . .
H68A H 0.867306 0.469857 0.692894 0.068 Uiso 1 1 calc GR . . . .
H68B H 0.753748 0.455505 0.685109 0.068 Uiso 1 1 calc GR . . . .
H68C H 0.791489 0.425567 0.745251 0.068 Uiso 1 1 calc GR . . . .
C69 C 0.7585(3) 0.6517(3) 0.90607(17) 0.0392(11) Uani 1 1 d . . . . .
H69 H 0.688031 0.675352 0.898178 0.047 Uiso 1 1 calc R . . . .
C70 C 0.7484(5) 0.5699(4) 0.9545(2) 0.0742(18) Uani 1 1 d . . . . .
H70A H 0.715418 0.525139 0.943214 0.111 Uiso 1 1 calc GR . . . .
H70B H 0.707313 0.586862 0.986866 0.111 Uiso 1 1 calc GR . . . .
H70C H 0.816181 0.545775 0.964184 0.111 Uiso 1 1 calc GR . . . .
C71 C 0.8049(4) 0.7217(4) 0.9236(2) 0.0515(13) Uani 1 1 d . . . . .
H71A H 0.866623 0.696387 0.940513 0.077 Uiso 1 1 calc GR . . . .
H71B H 0.756209 0.745959 0.950807 0.077 Uiso 1 1 calc GR . . . .
H71C H 0.822363 0.768814 0.891160 0.077 Uiso 1 1 calc GR . . . .
C72 C 0.5010(3) 0.6592(3) 0.68244(15) 0.0244(9) Uani 1 1 d . . . . .
C73 C 0.5192(3) 0.7125(3) 0.62889(15) 0.0272(9) Uani 1 1 d . . . . .
C74 C 0.4862(3) 0.6866(3) 0.58505(17) 0.0343(10) Uani 1 1 d . . . . .
H74 H 0.496533 0.722523 0.548668 0.041 Uiso 1 1 calc R . . . .
C75 C 0.4389(3) 0.6101(3) 0.59338(18) 0.0389(11) Uani 1 1 d . . . . .
H75 H 0.417603 0.593445 0.562774 0.047 Uiso 1 1 calc R . . . .
C76 C 0.4225(3) 0.5585(3) 0.64489(17) 0.0389(11) Uani 1 1 d . . . . .
H76 H 0.389964 0.505762 0.649904 0.047 Uiso 1 1 calc R . . . .
C77 C 0.4518(3) 0.5808(3) 0.69030(16) 0.0307(10) Uani 1 1 d . . . . .
C78 C 0.5694(3) 0.7977(3) 0.61789(15) 0.0279(9) Uani 1 1 d . . . . .
H78 H 0.602286 0.798183 0.651386 0.033 Uiso 1 1 calc R . . . .
C79 C 0.6513(3) 0.8067(3) 0.56833(15) 0.0348(11) Uani 1 1 d . . . . .
H79A H 0.700498 0.754902 0.573388 0.052 Uiso 1 1 calc GR . . . .
H79B H 0.686233 0.859805 0.565162 0.052 Uiso 1 1 calc GR . . . .
H79C H 0.620124 0.811181 0.534416 0.052 Uiso 1 1 calc GR . . . .
C80 C 0.4886(3) 0.8766(3) 0.60989(17) 0.0367(11) Uani 1 1 d . . . . .
H80A H 0.521316 0.931329 0.605076 0.055 Uiso 1 1 calc GR . . . .
H80B H 0.437281 0.870455 0.642623 0.055 Uiso 1 1 calc GR . . . .
H80C H 0.455951 0.878088 0.576877 0.055 Uiso 1 1 calc GR . . . .
C81 C 0.4314(3) 0.5224(3) 0.74812(17) 0.0373(11) Uani 1 1 d . . . . .
H81 H 0.450041 0.554620 0.775033 0.045 Uiso 1 1 calc R . . . .
C82 C 0.3197(4) 0.5058(4) 0.7641(2) 0.0627(16) Uani 1 1 d . . . . .
H82A H 0.277895 0.561846 0.756070 0.094 Uiso 1 1 calc GR . . . .
H82B H 0.307574 0.479030 0.803835 0.094 Uiso 1 1 calc GR . . . .
H82C H 0.301519 0.465986 0.742632 0.094 Uiso 1 1 calc GR . . . .
C83 C 0.4970(4) 0.4354(3) 0.7548(2) 0.0587(15) Uani 1 1 d . . . . .
H83A H 0.477154 0.399877 0.731054 0.088 Uiso 1 1 calc GR . . . .
H83B H 0.487404 0.403302 0.793665 0.088 Uiso 1 1 calc GR . . . .
H83C H 0.568732 0.446896 0.743958 0.088 Uiso 1 1 calc GR . . . .
C84 C 0.7075(3) 0.8277(3) 0.78237(15) 0.0217(9) Uani 1 1 d . . . . .
C85 C 1.2639(5) 0.2962(5) 0.9018(3) 0.100(3) Uani 1 1 d . . . . .
H85A H 1.278499 0.288340 0.940129 0.150 Uiso 1 1 calc GR . . . .
H85B H 1.306483 0.340092 0.877271 0.150 Uiso 1 1 calc GR . . . .
H85C H 1.278751 0.239930 0.890194 0.150 Uiso 1 1 calc GR . . . .
C86 C 1.1054(5) 0.4458(4) 0.9108(3) 0.0764(18) Uani 1 1 d . . . . .
H86A H 1.032913 0.465022 0.910657 0.115 Uiso 1 1 calc GR . . . .
H86B H 1.145226 0.486221 0.881631 0.115 Uiso 1 1 calc GR . . . .
H86C H 1.125854 0.445598 0.946994 0.115 Uiso 1 1 calc GR . . . .
C87 C 1.0951(5) 0.3359(5) 0.8285(3) 0.096(2) Uani 1 1 d . . . . .
H87A H 1.096757 0.275348 0.823670 0.144 Uiso 1 1 calc GR . . . .
H87B H 1.144068 0.368248 0.800040 0.144 Uiso 1 1 calc GR . . . .
H87C H 1.026603 0.364942 0.824934 0.144 Uiso 1 1 calc GR . . . .
C88 C 0.9177(4) 0.2786(4) 1.0405(2) 0.0590(15) Uani 1 1 d . . . . .
H88A H 0.969180 0.249143 1.064440 0.089 Uiso 1 1 calc GR . . . .
H88B H 0.850373 0.260964 1.058058 0.089 Uiso 1 1 calc GR . . . .
H88C H 0.918635 0.342582 1.034837 0.089 Uiso 1 1 calc GR . . . .
C89 C 0.8571(5) 0.3077(5) 0.9255(3) 0.088(2) Uani 1 1 d . . . . .
H89A H 0.855948 0.370863 0.924256 0.132 Uiso 1 1 calc GR . . . .
H89B H 0.788877 0.288033 0.938691 0.132 Uiso 1 1 calc GR . . . .
H89C H 0.878836 0.297055 0.888190 0.132 Uiso 1 1 calc GR . . . .
C90 C 0.9436(5) 0.1279(4) 0.9813(2) 0.0729(18) Uani 1 1 d . . . . .
H90A H 0.966237 0.111691 0.945547 0.109 Uiso 1 1 calc GR . . . .
H90B H 0.874156 0.111202 0.994523 0.109 Uiso 1 1 calc GR . . . .
H90C H 0.989148 0.097144 1.008431 0.109 Uiso 1 1 calc GR . . . .
C91 C 0.1544(4) 0.6355(3) 0.6218(2) 0.0572(14) Uani 1 1 d . . . . .
H91A H 0.209568 0.624757 0.645266 0.086 Uiso 1 1 calc GR . . . .
H91B H 0.091399 0.655335 0.642594 0.086 Uiso 1 1 calc GR . . . .
H91C H 0.171934 0.680928 0.588445 0.086 Uiso 1 1 calc GR . . . .
C92 C 0.0233(4) 0.5461(5) 0.5662(2) 0.081(2) Uani 1 1 d . . . . .
H92A H 0.030415 0.593372 0.532683 0.122 Uiso 1 1 calc GR . . . .
H92B H -0.036918 0.560655 0.590995 0.122 Uiso 1 1 calc GR . . . .
H92C H 0.015788 0.490715 0.555734 0.122 Uiso 1 1 calc GR . . . .
C93 C 0.1245(4) 0.4419(4) 0.6651(2) 0.0609(15) Uani 1 1 d . . . . .
H93A H 0.108389 0.388752 0.654762 0.091 Uiso 1 1 calc GR . . . .
H93B H 0.069940 0.458761 0.692473 0.091 Uiso 1 1 calc GR . . . .
H93C H 0.188805 0.430031 0.681237 0.091 Uiso 1 1 calc GR . . . .
C94 C 0.4099(3) 0.3885(3) 0.55228(17) 0.0386(11) Uani 1 1 d . . . . .
H94A H 0.454766 0.435970 0.547160 0.058 Uiso 1 1 calc GR . . . .
H94B H 0.442184 0.344494 0.531593 0.058 Uiso 1 1 calc GR . . . .
H94C H 0.397431 0.360688 0.591857 0.058 Uiso 1 1 calc GR . . . .
C95 C 0.2049(4) 0.3436(3) 0.5363(2) 0.0470(13) Uani 1 1 d . . . . .
H95A H 0.193825 0.315193 0.575784 0.071 Uiso 1 1 calc GR . . . .
H95B H 0.237396 0.300310 0.515080 0.071 Uiso 1 1 calc GR . . . .
H95C H 0.139395 0.367291 0.523140 0.071 Uiso 1 1 calc GR . . . .
C96 C 0.3060(4) 0.4920(3) 0.45236(17) 0.0443(12) Uani 1 1 d . . . . .
H96A H 0.239615 0.514759 0.440069 0.066 Uiso 1 1 calc GR . . . .
H96B H 0.339529 0.450811 0.429916 0.066 Uiso 1 1 calc GR . . . .
H96C H 0.348300 0.541109 0.447919 0.066 Uiso 1 1 calc GR . . . .
N1 N 0.6240(2) 1.1391(2) 0.68527(11) 0.0192(7) Uani 1 1 d . . . . .
N2 N 0.7284(2) 1.0940(2) 0.78471(11) 0.0200(7) Uani 1 1 d . . . . .
N3 N 0.8277(2) 1.0375(2) 0.68023(12) 0.0224(7) Uani 1 1 d . . . . .
N4 N 0.4487(2) 0.6972(2) 0.84484(12) 0.0271(8) Uani 1 1 d . . . . .
N5 N 0.6511(2) 0.6153(2) 0.82124(12) 0.0248(7) Uani 1 1 d . . . . .
N6 N 0.5291(2) 0.6850(2) 0.72795(12) 0.0232(7) Uani 1 1 d . . . . .
O1 O 0.62429(18) 0.95077(16) 0.69000(9) 0.0199(6) Uani 1 1 d . . . . .
O2 O 0.55572(18) 0.97943(17) 0.76965(10) 0.0242(6) Uani 1 1 d . . . . .
O3 O 0.51145(18) 0.86138(16) 0.74437(10) 0.0210(5) Uani 1 1 d . . . . .
O4 O 0.64788(19) 0.80783(17) 0.82664(10) 0.0250(6) Uani 1 1 d . . . . .
O5 O 0.70825(18) 0.78000(16) 0.74589(10) 0.0211(6) Uani 1 1 d . . . . .
O6 O 0.75838(18) 0.89665(16) 0.77023(9) 0.0204(6) Uani 1 1 d . . . . .
O7 O 1.0625(3) 0.2698(3) 0.94668(14) 0.0616(10) Uani 1 1 d . . . . .
O8 O 0.2366(2) 0.5068(2) 0.56137(12) 0.0407(8) Uani 1 1 d . . . . .
Nb1 Nb 0.71162(2) 1.01997(2) 0.72555(2) 0.01810(11) Uani 1 1 d . . . . .
Nb2 Nb 0.56635(2) 0.73425(2) 0.77855(2) 0.02001(11) Uani 1 1 d . . . . .
Si1 Si 1.12853(12) 0.33404(12) 0.89763(6) 0.0643(5) Uani 1 1 d . . . . .
Si2 Si 0.94606(10) 0.24681(10) 0.97272(5) 0.0436(3) Uani 1 1 d . . . . .
Si3 Si 0.13658(9) 0.53382(9) 0.60181(5) 0.0399(3) Uani 1 1 d . . . . .
Si4 Si 0.28802(8) 0.43434(8) 0.52636(5) 0.0279(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.407(5) . ?
C1 C4 1.487(5) . ?
C1 N1 1.327(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.398(5) . ?
C3 C5 1.507(5) . ?
C3 N2 1.345(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.407(5) . ?
C6 C11 1.412(5) . ?
C6 N1 1.455(5) . ?
C7 C8 1.405(5) . ?
C7 C12 1.516(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.363(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.391(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.391(6) . ?
C11 C15 1.513(5) . ?
C12 H12 1.0000 . ?
C12 C13 1.537(5) . ?
C12 C14 1.522(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.538(6) . ?
C15 C17 1.522(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.398(5) . ?
C18 C23 1.404(5) . ?
C18 N2 1.449(4) . ?
C19 C20 1.378(5) . ?
C19 C24 1.527(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.380(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.377(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.387(5) . ?
C23 C27 1.518(5) . ?
C24 H24 1.0000 . ?
C24 C25 1.511(6) . ?
C24 C26 1.539(6) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27 1.0000 . ?
C27 C28 1.512(7) . ?
C27 C29 1.541(6) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.414(6) . ?
C30 C35 1.417(6) . ?
C30 N3 1.405(5) . ?
C31 C32 1.392(6) . ?
C31 C36 1.502(6) . ?
C32 H32 0.9500 . ?
C32 C33 1.347(6) . ?
C33 H33 0.9500 . ?
C33 C34 1.381(7) . ?
C34 H34 0.9500 . ?
C34 C35 1.387(5) . ?
C35 C39 1.502(6) . ?
C36 H36 1.0000 . ?
C36 C37 1.516(8) . ?
C36 C38 1.512(8) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39 1.0000 . ?
C39 C40 1.539(5) . ?
C39 C41 1.534(6) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 O1 1.313(4) . ?
C42 O2 1.255(4) . ?
C42 O3 1.293(4) . ?
C42 Nb1 2.529(4) . ?
C43 C44 1.391(6) . ?
C43 C46 1.510(5) . ?
C43 N4 1.341(5) . ?
C44 H44 0.9500 . ?
C44 C45 1.413(6) . ?
C45 C47 1.495(6) . ?
C45 N5 1.315(5) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C49 1.400(6) . ?
C48 C53 1.398(6) . ?
C48 N4 1.461(5) . ?
C49 C50 1.392(6) . ?
C49 C54 1.514(6) . ?
C50 H50 0.9500 . ?
C50 C51 1.363(6) . ?
C51 H51 0.9500 . ?
C51 C52 1.379(6) . ?
C52 H52 0.9500 . ?
C52 C53 1.380(6) . ?
C53 C57 1.518(6) . ?
C54 H54 1.0000 . ?
C54 C55 1.516(7) . ?
C54 C56 1.538(6) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57 1.0000 . ?
C57 C58 1.530(7) . ?
C57 C59 1.534(6) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 C61 1.405(5) . ?
C60 C65 1.399(6) . ?
C60 N5 1.453(5) . ?
C61 C62 1.381(6) . ?
C61 C66 1.528(6) . ?
C62 H62 0.9500 . ?
C62 C63 1.379(7) . ?
C63 H63 0.9500 . ?
C63 C64 1.379(6) . ?
C64 H64 0.9500 . ?
C64 C65 1.377(6) . ?
C65 C69 1.511(6) . ?
C66 H66 1.0000 . ?
C66 C67 1.529(6) . ?
C66 C68 1.529(6) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 H69 1.0000 . ?
C69 C70 1.546(6) . ?
C69 C71 1.494(6) . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 C73 1.404(5) . ?
C72 C77 1.418(6) . ?
C72 N6 1.400(5) . ?
C73 C74 1.392(5) . ?
C73 C78 1.510(6) . ?
C74 H74 0.9500 . ?
C74 C75 1.376(6) . ?
C75 H75 0.9500 . ?
C75 C76 1.351(6) . ?
C76 H76 0.9500 . ?
C76 C77 1.378(6) . ?
C77 C81 1.523(6) . ?
C78 H78 1.0000 . ?
C78 C79 1.517(5) . ?
C78 C80 1.541(6) . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 H81 1.0000 . ?
C81 C82 1.520(6) . ?
C81 C83 1.523(7) . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 O4 1.260(4) . ?
C84 O5 1.303(4) . ?
C84 O6 1.292(4) . ?
C84 Nb2 2.535(4) . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C85 Si1 1.846(6) . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C86 Si1 1.838(6) . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C87 Si1 1.835(7) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C88 Si2 1.846(5) . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C89 Si2 1.825(6) . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
C90 Si2 1.827(6) . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
C91 Si3 1.824(5) . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C92 Si3 1.831(5) . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?
C93 Si3 1.875(5) . ?
C94 H94A 0.9800 . ?
C94 H94B 0.9800 . ?
C94 H94C 0.9800 . ?
C94 Si4 1.843(4) . ?
C95 H95A 0.9800 . ?
C95 H95B 0.9800 . ?
C95 H95C 0.9800 . ?
C95 Si4 1.849(5) . ?
C96 H96A 0.9800 . ?
C96 H96B 0.9800 . ?
C96 H96C 0.9800 . ?
C96 Si4 1.851(4) . ?
N1 Nb1 2.199(3) . ?
N2 Nb1 2.125(3) . ?
N3 Nb1 1.787(3) . ?
N4 Nb2 2.129(3) . ?
N5 Nb2 2.199(3) . ?
N6 Nb2 1.775(3) . ?
O1 Nb1 2.084(2) . ?
O2 Nb1 2.289(2) . ?
O3 Nb2 2.071(2) . ?
O4 Nb2 2.291(3) . ?
O5 Nb2 2.084(2) . ?
O6 Nb1 2.071(2) . ?
O7 Si1 1.612(4) . ?
O7 Si2 1.639(4) . ?
O8 Si3 1.629(3) . ?
O8 Si4 1.623(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C4 115.2(4) . . ?
N1 C1 C2 123.6(4) . . ?
N1 C1 C4 121.2(3) . . ?
C1 C2 H2 115.4 . . ?
C3 C2 C1 129.2(4) . . ?
C3 C2 H2 115.4 . . ?
C2 C3 C5 116.0(4) . . ?
N2 C3 C2 123.4(3) . . ?
N2 C3 C5 120.6(3) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 121.3(3) . . ?
C7 C6 N1 118.8(3) . . ?
C11 C6 N1 119.9(3) . . ?
C6 C7 C12 123.0(3) . . ?
C8 C7 C6 117.8(3) . . ?
C8 C7 C12 119.2(3) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 C7 121.3(4) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 H9 119.8 . . ?
C8 C9 C10 120.5(4) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 119.5 . . ?
C9 C10 C11 120.9(4) . . ?
C11 C10 H10 119.5 . . ?
C6 C11 C15 123.5(3) . . ?
C10 C11 C6 118.1(3) . . ?
C10 C11 C15 118.3(3) . . ?
C7 C12 H12 107.9 . . ?
C7 C12 C13 111.7(3) . . ?
C7 C12 C14 111.1(3) . . ?
C13 C12 H12 107.9 . . ?
C14 C12 H12 107.9 . . ?
C14 C12 C13 110.2(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15 107.7 . . ?
C11 C15 C16 110.5(3) . . ?
C11 C15 C17 113.3(4) . . ?
C16 C15 H15 107.7 . . ?
C17 C15 H15 107.7 . . ?
C17 C15 C16 109.7(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 121.5(3) . . ?
C19 C18 N2 118.7(3) . . ?
C23 C18 N2 119.7(3) . . ?
C18 C19 C24 121.3(3) . . ?
C20 C19 C18 118.1(4) . . ?
C20 C19 C24 120.6(3) . . ?
C19 C20 H20 119.0 . . ?
C19 C20 C21 122.0(4) . . ?
C21 C20 H20 119.0 . . ?
C20 C21 H21 120.6 . . ?
C22 C21 C20 118.8(4) . . ?
C22 C21 H21 120.6 . . ?
C21 C22 H22 118.9 . . ?
C21 C22 C23 122.1(4) . . ?
C23 C22 H22 118.9 . . ?
C18 C23 C27 123.7(3) . . ?
C22 C23 C18 117.4(4) . . ?
C22 C23 C27 118.9(4) . . ?
C19 C24 H24 107.7 . . ?
C19 C24 C26 110.9(4) . . ?
C25 C24 C19 112.4(4) . . ?
C25 C24 H24 107.7 . . ?
C25 C24 C26 110.2(4) . . ?
C26 C24 H24 107.7 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27 107.5 . . ?
C23 C27 C29 110.6(4) . . ?
C28 C27 C23 113.1(4) . . ?
C28 C27 H27 107.5 . . ?
C28 C27 C29 110.2(4) . . ?
C29 C27 H27 107.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C35 120.7(4) . . ?
N3 C30 C31 119.8(4) . . ?
N3 C30 C35 119.5(4) . . ?
C30 C31 C36 122.3(4) . . ?
C32 C31 C30 117.4(4) . . ?
C32 C31 C36 120.3(4) . . ?
C31 C32 H32 118.7 . . ?
C33 C32 C31 122.7(4) . . ?
C33 C32 H32 118.7 . . ?
C32 C33 H33 120.1 . . ?
C32 C33 C34 119.8(4) . . ?
C34 C33 H33 120.1 . . ?
C33 C34 H34 119.1 . . ?
C33 C34 C35 121.7(4) . . ?
C35 C34 H34 119.1 . . ?
C30 C35 C39 122.3(3) . . ?
C34 C35 C30 117.7(4) . . ?
C34 C35 C39 119.9(4) . . ?
C31 C36 H36 107.4 . . ?
C31 C36 C37 112.7(5) . . ?
C31 C36 C38 111.1(5) . . ?
C37 C36 H36 107.4 . . ?
C38 C36 H36 107.4 . . ?
C38 C36 C37 110.7(4) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C39 H39 108.0 . . ?
C35 C39 C40 111.8(3) . . ?
C35 C39 C41 111.1(3) . . ?
C40 C39 H39 108.0 . . ?
C41 C39 H39 108.0 . . ?
C41 C39 C40 109.9(3) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O1 C42 Nb1 55.35(17) . . ?
O2 C42 O1 116.6(3) . . ?
O2 C42 O3 123.9(3) . . ?
O2 C42 Nb1 64.53(19) . . ?
O3 C42 O1 119.3(3) . . ?
O3 C42 Nb1 157.1(3) . . ?
C44 C43 C46 116.4(4) . . ?
N4 C43 C44 123.3(4) . . ?
N4 C43 C46 120.2(4) . . ?
C43 C44 H44 115.8 . . ?
C43 C44 C45 128.3(4) . . ?
C45 C44 H44 115.8 . . ?
C44 C45 C47 114.9(4) . . ?
N5 C45 C44 123.6(4) . . ?
N5 C45 C47 121.5(4) . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C49 C48 N4 118.6(3) . . ?
C53 C48 C49 121.8(4) . . ?
C53 C48 N4 119.6(4) . . ?
C48 C49 C54 122.8(4) . . ?
C50 C49 C48 117.6(4) . . ?
C50 C49 C54 119.6(4) . . ?
C49 C50 H50 119.4 . . ?
C51 C50 C49 121.2(4) . . ?
C51 C50 H50 119.4 . . ?
C50 C51 H51 119.9 . . ?
C50 C51 C52 120.2(4) . . ?
C52 C51 H51 119.9 . . ?
C51 C52 H52 119.3 . . ?
C51 C52 C53 121.4(4) . . ?
C53 C52 H52 119.3 . . ?
C48 C53 C57 123.0(4) . . ?
C52 C53 C48 117.7(4) . . ?
C52 C53 C57 119.2(4) . . ?
C49 C54 H54 107.5 . . ?
C49 C54 C55 111.3(4) . . ?
C49 C54 C56 112.3(4) . . ?
C55 C54 H54 107.5 . . ?
C55 C54 C56 110.4(4) . . ?
C56 C54 H54 107.5 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C53 C57 H57 108.3 . . ?
C53 C57 C58 112.0(4) . . ?
C53 C57 C59 111.0(4) . . ?
C58 C57 H57 108.3 . . ?
C58 C57 C59 108.9(4) . . ?
C59 C57 H57 108.3 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C61 C60 N5 119.3(4) . . ?
C65 C60 C61 121.1(4) . . ?
C65 C60 N5 119.6(3) . . ?
C60 C61 C66 122.8(4) . . ?
C62 C61 C60 118.7(4) . . ?
C62 C61 C66 118.4(4) . . ?
C61 C62 H62 119.9 . . ?
C63 C62 C61 120.2(4) . . ?
C63 C62 H62 119.9 . . ?
C62 C63 H63 119.7 . . ?
C64 C63 C62 120.7(4) . . ?
C64 C63 H63 119.7 . . ?
C63 C64 H64 119.5 . . ?
C65 C64 C63 121.0(4) . . ?
C65 C64 H64 119.5 . . ?
C60 C65 C69 121.7(4) . . ?
C64 C65 C60 118.3(4) . . ?
C64 C65 C69 120.0(4) . . ?
C61 C66 H66 108.0 . . ?
C61 C66 C67 110.6(4) . . ?
C61 C66 C68 112.5(4) . . ?
C67 C66 H66 108.0 . . ?
C67 C66 C68 109.6(3) . . ?
C68 C66 H66 108.0 . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C66 C68 H68A 109.5 . . ?
C66 C68 H68B 109.5 . . ?
C66 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C65 C69 H69 107.1 . . ?
C65 C69 C70 111.4(4) . . ?
C70 C69 H69 107.1 . . ?
C71 C69 C65 113.8(4) . . ?
C71 C69 H69 107.1 . . ?
C71 C69 C70 109.9(4) . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C69 C71 H71A 109.5 . . ?
C69 C71 H71B 109.5 . . ?
C69 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C73 C72 C77 119.7(3) . . ?
N6 C72 C73 119.9(3) . . ?
N6 C72 C77 120.3(3) . . ?
C72 C73 C78 122.3(3) . . ?
C74 C73 C72 118.2(4) . . ?
C74 C73 C78 119.4(4) . . ?
C73 C74 H74 119.4 . . ?
C75 C74 C73 121.3(4) . . ?
C75 C74 H74 119.4 . . ?
C74 C75 H75 119.8 . . ?
C76 C75 C74 120.3(4) . . ?
C76 C75 H75 119.8 . . ?
C75 C76 H76 119.3 . . ?
C75 C76 C77 121.5(4) . . ?
C77 C76 H76 119.3 . . ?
C72 C77 C81 120.4(3) . . ?
C76 C77 C72 119.0(4) . . ?
C76 C77 C81 120.7(4) . . ?
C73 C78 H78 107.9 . . ?
C73 C78 C79 112.5(3) . . ?
C73 C78 C80 110.0(3) . . ?
C79 C78 H78 107.9 . . ?
C79 C78 C80 110.5(3) . . ?
C80 C78 H78 107.9 . . ?
C78 C79 H79A 109.5 . . ?
C78 C79 H79B 109.5 . . ?
C78 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C78 C80 H80A 109.5 . . ?
C78 C80 H80B 109.5 . . ?
C78 C80 H80C 109.5 . . ?
H80A C80 H80B 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C77 C81 H81 107.2 . . ?
C82 C81 C77 112.3(4) . . ?
C82 C81 H81 107.2 . . ?
C82 C81 C83 110.3(4) . . ?
C83 C81 C77 112.4(4) . . ?
C83 C81 H81 107.2 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C81 C83 H83A 109.5 . . ?
C81 C83 H83B 109.5 . . ?
C81 C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
O4 C84 O5 116.5(3) . . ?
O4 C84 O6 123.0(3) . . ?
O4 C84 Nb2 64.3(2) . . ?
O5 C84 Nb2 55.06(17) . . ?
O6 C84 O5 120.1(3) . . ?
O6 C84 Nb2 157.0(3) . . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
Si1 C85 H85A 109.5 . . ?
Si1 C85 H85B 109.5 . . ?
Si1 C85 H85C 109.5 . . ?
H86A C86 H86B 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
Si1 C86 H86A 109.5 . . ?
Si1 C86 H86B 109.5 . . ?
Si1 C86 H86C 109.5 . . ?
H87A C87 H87B 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
Si1 C87 H87A 109.5 . . ?
Si1 C87 H87B 109.5 . . ?
Si1 C87 H87C 109.5 . . ?
H88A C88 H88B 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
Si2 C88 H88A 109.5 . . ?
Si2 C88 H88B 109.5 . . ?
Si2 C88 H88C 109.5 . . ?
H89A C89 H89B 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
Si2 C89 H89A 109.5 . . ?
Si2 C89 H89B 109.5 . . ?
Si2 C89 H89C 109.5 . . ?
H90A C90 H90B 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
Si2 C90 H90A 109.5 . . ?
Si2 C90 H90B 109.5 . . ?
Si2 C90 H90C 109.5 . . ?
H91A C91 H91B 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
Si3 C91 H91A 109.5 . . ?
Si3 C91 H91B 109.5 . . ?
Si3 C91 H91C 109.5 . . ?
H92A C92 H92B 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
Si3 C92 H92A 109.5 . . ?
Si3 C92 H92B 109.5 . . ?
Si3 C92 H92C 109.5 . . ?
H93A C93 H93B 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
Si3 C93 H93A 109.5 . . ?
Si3 C93 H93B 109.5 . . ?
Si3 C93 H93C 109.5 . . ?
H94A C94 H94B 109.5 . . ?
H94A C94 H94C 109.5 . . ?
H94B C94 H94C 109.5 . . ?
Si4 C94 H94A 109.5 . . ?
Si4 C94 H94B 109.5 . . ?
Si4 C94 H94C 109.5 . . ?
H95A C95 H95B 109.5 . . ?
H95A C95 H95C 109.5 . . ?
H95B C95 H95C 109.5 . . ?
Si4 C95 H95A 109.5 . . ?
Si4 C95 H95B 109.5 . . ?
Si4 C95 H95C 109.5 . . ?
H96A C96 H96B 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
Si4 C96 H96A 109.5 . . ?
Si4 C96 H96B 109.5 . . ?
Si4 C96 H96C 109.5 . . ?
C1 N1 C6 117.1(3) . . ?
C1 N1 Nb1 121.8(2) . . ?
C6 N1 Nb1 120.4(2) . . ?
C3 N2 C18 116.7(3) . . ?
C3 N2 Nb1 123.2(2) . . ?
C18 N2 Nb1 120.1(2) . . ?
C30 N3 Nb1 173.0(3) . . ?
C43 N4 C48 118.4(3) . . ?
C43 N4 Nb2 124.9(3) . . ?
C48 N4 Nb2 116.7(2) . . ?
C45 N5 C60 116.4(3) . . ?
C45 N5 Nb2 122.8(3) . . ?
C60 N5 Nb2 120.1(2) . . ?
C72 N6 Nb2 171.0(3) . . ?
C42 O1 Nb1 93.4(2) . . ?
C42 O2 Nb1 85.8(2) . . ?
C42 O3 Nb2 126.0(2) . . ?
C84 O4 Nb2 85.9(2) . . ?
C84 O5 Nb2 94.1(2) . . ?
C84 O6 Nb1 126.0(2) . . ?
Si1 O7 Si2 143.4(2) . . ?
Si4 O8 Si3 144.6(2) . . ?
N1 Nb1 C42 90.40(11) . . ?
N1 Nb1 O2 84.00(10) . . ?
N2 Nb1 C42 121.76(11) . . ?
N2 Nb1 N1 85.07(11) . . ?
N2 Nb1 O2 92.29(10) . . ?
N3 Nb1 C42 137.33(13) . . ?
N3 Nb1 N1 96.73(12) . . ?
N3 Nb1 N2 100.79(13) . . ?
N3 Nb1 O1 107.21(12) . . ?
N3 Nb1 O2 166.92(12) . . ?
N3 Nb1 O6 96.43(12) . . ?
O1 Nb1 C42 31.22(10) . . ?
O1 Nb1 N1 86.06(11) . . ?
O1 Nb1 N2 151.41(10) . . ?
O1 Nb1 O2 59.75(9) . . ?
O2 Nb1 C42 29.67(10) . . ?
O6 Nb1 C42 76.03(11) . . ?
O6 Nb1 N1 165.66(10) . . ?
O6 Nb1 N2 98.04(10) . . ?
O6 Nb1 O1 84.62(9) . . ?
O6 Nb1 O2 81.90(9) . . ?
N4 Nb2 C84 124.32(12) . . ?
N4 Nb2 N5 83.93(12) . . ?
N4 Nb2 O4 94.65(11) . . ?
N5 Nb2 C84 90.85(12) . . ?
N5 Nb2 O4 85.37(11) . . ?
N6 Nb2 C84 135.75(13) . . ?
N6 Nb2 N4 99.90(13) . . ?
N6 Nb2 N5 95.72(13) . . ?
N6 Nb2 O3 95.92(12) . . ?
N6 Nb2 O4 165.45(11) . . ?
N6 Nb2 O5 105.99(12) . . ?
O3 Nb2 C84 76.02(11) . . ?
O3 Nb2 N4 100.75(11) . . ?
O3 Nb2 N5 166.51(11) . . ?
O3 Nb2 O4 81.65(9) . . ?
O3 Nb2 O5 84.22(9) . . ?
O4 Nb2 C84 29.73(10) . . ?
O5 Nb2 C84 30.85(10) . . ?
O5 Nb2 N4 153.02(11) . . ?
O5 Nb2 N5 86.03(11) . . ?
O5 Nb2 O4 59.55(9) . . ?
C86 Si1 C85 109.0(3) . . ?
C87 Si1 C85 110.5(3) . . ?
C87 Si1 C86 109.2(3) . . ?
O7 Si1 C85 107.5(3) . . ?
O7 Si1 C86 107.7(3) . . ?
O7 Si1 C87 112.8(3) . . ?
C89 Si2 C88 110.2(3) . . ?
C89 Si2 C90 111.5(3) . . ?
C90 Si2 C88 110.9(3) . . ?
O7 Si2 C88 108.3(2) . . ?
O7 Si2 C89 109.7(3) . . ?
O7 Si2 C90 106.2(2) . . ?
C91 Si3 C92 111.2(3) . . ?
C91 Si3 C93 109.6(2) . . ?
C92 Si3 C93 109.6(3) . . ?
O8 Si3 C91 109.5(2) . . ?
O8 Si3 C92 109.7(2) . . ?
O8 Si3 C93 107.1(2) . . ?
C94 Si4 C95 108.7(2) . . ?
C94 Si4 C96 112.0(2) . . ?
C95 Si4 C96 110.3(2) . . ?
O8 Si4 C94 108.23(18) . . ?
O8 Si4 C95 110.64(19) . . ?
O8 Si4 C96 107.0(2) . . ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bmkxr71
_database_code_depnum_ccdc_archive 'CCDC 2004137'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-14 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_audit_creation_date             2020-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            (BDI)Nb(OCHNtBu)(O[SiMe2Ph])(NAr)
_chemical_name_systematic        
(2,6-diisopropylphenyl)imino-(tert-butyliminomethoxy)-dimethylphenylsilanolato-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V)
_chemical_formula_moiety         'C54 H79 N4 Nb O2 Si'
_chemical_formula_sum            'C54 H79 N4 Nb O2 Si'
_chemical_formula_weight         937.21
_chemical_melting_point          478
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.629(2)
_cell_length_b                   21.336(4)
_cell_length_c                   19.715(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.431(4)
_cell_angle_gamma                90
_cell_volume                     5307.4(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.17
_shelx_estimated_absorpt_T_max   0.977
_shelx_estimated_absorpt_T_min   0.966
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6620
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0556 before and 0.0471 after correction.
The Ratio of minimum to maximum transmission is 0.8884.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59328
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.389
_diffrn_reflns_theta_min         1.407
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8048
_reflns_number_total             9689
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         9689
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0453
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0422P)²+7.8592P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1082
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C36(H36), C39(H39)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32),
 C33(H33), C34(H34), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C50(H50)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C48(H48A,H48B,H48C),
 C49(H49A,H49B,H49C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6534(2) 0.68754(13) 0.26279(14) 0.0195(6) Uani 1 1 d . . . . .
C2 C 0.7180(2) 0.73107(13) 0.23221(14) 0.0204(6) Uani 1 1 d . . . . .
H2 H 0.738994 0.720922 0.187831 0.024 Uiso 1 1 calc R . . . .
C3 C 0.7557(2) 0.78780(13) 0.25874(14) 0.0188(6) Uani 1 1 d . . . . .
C4 C 0.6051(3) 0.63756(14) 0.21710(15) 0.0289(7) Uani 1 1 d . . . . .
H4A H 0.633934 0.596553 0.230573 0.043 Uiso 1 1 calc GR . . . .
H4B H 0.621993 0.646286 0.169967 0.043 Uiso 1 1 calc GR . . . .
H4C H 0.528011 0.637352 0.221060 0.043 Uiso 1 1 calc GR . . . .
C5 C 0.7987(3) 0.83330(14) 0.20776(14) 0.0274(7) Uani 1 1 d . . . . .
H5A H 0.767034 0.874715 0.214129 0.041 Uiso 1 1 calc GR . . . .
H5B H 0.780968 0.818391 0.161649 0.041 Uiso 1 1 calc GR . . . .
H5C H 0.875846 0.836249 0.214513 0.041 Uiso 1 1 calc GR . . . .
C6 C 0.5440(2) 0.64899(13) 0.34852(13) 0.0203(6) Uani 1 1 d . . . . .
C7 C 0.5653(2) 0.58773(13) 0.37090(14) 0.0224(6) Uani 1 1 d . . . . .
C8 C 0.4794(3) 0.55118(14) 0.38981(15) 0.0292(7) Uani 1 1 d . . . . .
H8 H 0.491603 0.509496 0.405147 0.035 Uiso 1 1 calc R . . . .
C9 C 0.3770(3) 0.57441(16) 0.38666(18) 0.0371(8) Uani 1 1 d . . . . .
H9 H 0.320074 0.548819 0.400175 0.044 Uiso 1 1 calc R . . . .
C10 C 0.3574(3) 0.63459(15) 0.36395(17) 0.0319(7) Uani 1 1 d . . . . .
H10 H 0.286876 0.650209 0.361960 0.038 Uiso 1 1 calc R . . . .
C11 C 0.4402(2) 0.67279(14) 0.34387(14) 0.0232(6) Uani 1 1 d . . . . .
C12 C 0.6766(2) 0.55987(13) 0.37522(14) 0.0235(6) Uani 1 1 d . . . . .
H12 H 0.725768 0.590680 0.354902 0.028 Uiso 1 1 calc R . . . .
C13 C 0.6833(3) 0.49839(14) 0.33535(17) 0.0350(8) Uani 1 1 d . . . . .
H13A H 0.638547 0.466679 0.355904 0.053 Uiso 1 1 calc GR . . . .
H13B H 0.756886 0.483772 0.336514 0.053 Uiso 1 1 calc GR . . . .
H13C H 0.658659 0.505434 0.288155 0.053 Uiso 1 1 calc GR . . . .
C14 C 0.7145(3) 0.54874(15) 0.44910(15) 0.0297(7) Uani 1 1 d . . . . .
H14A H 0.710569 0.588076 0.474538 0.044 Uiso 1 1 calc GR . . . .
H14B H 0.787878 0.533763 0.450444 0.044 Uiso 1 1 calc GR . . . .
H14C H 0.669177 0.517267 0.469566 0.044 Uiso 1 1 calc GR . . . .
C15 C 0.4148(2) 0.73779(14) 0.31523(15) 0.0241(6) Uani 1 1 d . . . . .
H15 H 0.482773 0.757926 0.302778 0.029 Uiso 1 1 calc R . . . .
C16 C 0.3422(3) 0.73379(18) 0.25123(17) 0.0441(9) Uani 1 1 d . . . . .
H16A H 0.275596 0.713334 0.262158 0.066 Uiso 1 1 calc GR . . . .
H16B H 0.377218 0.709361 0.216536 0.066 Uiso 1 1 calc GR . . . .
H16C H 0.327402 0.776111 0.234002 0.066 Uiso 1 1 calc GR . . . .
C17 C 0.3620(3) 0.78002(17) 0.36581(17) 0.0394(8) Uani 1 1 d . . . . .
H17A H 0.295402 0.760875 0.379073 0.059 Uiso 1 1 calc GR . . . .
H17B H 0.347183 0.820938 0.344905 0.059 Uiso 1 1 calc GR . . . .
H17C H 0.409226 0.785493 0.406097 0.059 Uiso 1 1 calc GR . . . .
C18 C 0.7859(2) 0.86660(12) 0.34211(13) 0.0180(6) Uani 1 1 d . . . . .
C19 C 0.7063(2) 0.91118(13) 0.35250(13) 0.0195(6) Uani 1 1 d . . . . .
C20 C 0.7387(2) 0.97212(13) 0.36881(14) 0.0246(7) Uani 1 1 d . . . . .
H20 H 0.686822 1.003694 0.374536 0.030 Uiso 1 1 calc R . . . .
C21 C 0.8456(2) 0.98749(14) 0.37684(15) 0.0264(7) Uani 1 1 d . . . . .
H21 H 0.866025 1.029191 0.388072 0.032 Uiso 1 1 calc R . . . .
C22 C 0.9212(3) 0.94261(14) 0.36856(15) 0.0272(7) Uani 1 1 d . . . . .
H22 H 0.993799 0.953477 0.375228 0.033 Uiso 1 1 calc R . . . .
C23 C 0.8942(2) 0.88111(13) 0.35053(14) 0.0217(6) Uani 1 1 d . . . . .
C24 C 0.5887(2) 0.89443(14) 0.34678(15) 0.0239(6) Uani 1 1 d . . . . .
H24 H 0.582157 0.849802 0.361514 0.029 Uiso 1 1 calc R . . . .
C25 C 0.5221(3) 0.93379(16) 0.39363(18) 0.0355(8) Uani 1 1 d . . . . .
H25A H 0.554599 0.933187 0.439664 0.053 Uiso 1 1 calc GR . . . .
H25B H 0.450349 0.916387 0.394320 0.053 Uiso 1 1 calc GR . . . .
H25C H 0.518652 0.977051 0.376991 0.053 Uiso 1 1 calc GR . . . .
C26 C 0.5449(3) 0.89817(16) 0.27354(17) 0.0365(8) Uani 1 1 d . . . . .
H26A H 0.469098 0.888130 0.271939 0.055 Uiso 1 1 calc GR . . . .
H26B H 0.582370 0.868143 0.245589 0.055 Uiso 1 1 calc GR . . . .
H26C H 0.555057 0.940652 0.256060 0.055 Uiso 1 1 calc GR . . . .
C27 C 0.9820(2) 0.83367(14) 0.34165(16) 0.0269(7) Uani 1 1 d . . . . .
H27 H 0.949541 0.795588 0.319754 0.032 Uiso 1 1 calc R . . . .
C28 C 1.0685(3) 0.85802(16) 0.29500(18) 0.0359(8) Uani 1 1 d . . . . .
H28A H 1.035182 0.873201 0.252311 0.054 Uiso 1 1 calc GR . . . .
H28B H 1.117651 0.823896 0.285476 0.054 Uiso 1 1 calc GR . . . .
H28C H 1.107453 0.892373 0.317674 0.054 Uiso 1 1 calc GR . . . .
C29 C 1.0322(2) 0.81375(16) 0.41041(17) 0.0331(8) Uani 1 1 d . . . . .
H29A H 1.068754 0.849632 0.431783 0.050 Uiso 1 1 calc GR . . . .
H29B H 1.083170 0.779930 0.403649 0.050 Uiso 1 1 calc GR . . . .
H29C H 0.976712 0.798947 0.439789 0.050 Uiso 1 1 calc GR . . . .
C30 C 0.9241(2) 0.65104(14) 0.42364(15) 0.0244(7) Uani 1 1 d . . . . .
C31 C 0.9742(2) 0.62653(14) 0.36679(16) 0.0278(7) Uani 1 1 d . . . . .
C32 C 1.0581(3) 0.58452(18) 0.37821(19) 0.0467(10) Uani 1 1 d . . . . .
H32 H 1.092952 0.567788 0.340492 0.056 Uiso 1 1 calc R . . . .
C33 C 1.0910(3) 0.5669(2) 0.4424(2) 0.0635(13) Uani 1 1 d . . . . .
H33 H 1.147481 0.537839 0.448753 0.076 Uiso 1 1 calc R . . . .
C34 C 1.0424(3) 0.5913(2) 0.4978(2) 0.0590(13) Uani 1 1 d . . . . .
H34 H 1.066483 0.578973 0.542135 0.071 Uiso 1 1 calc R . . . .
C35 C 0.9589(3) 0.63366(17) 0.49026(17) 0.0358(8) Uani 1 1 d . . . . .
C36 C 0.9420(2) 0.64567(14) 0.29479(15) 0.0266(7) Uani 1 1 d . . . . .
H36 H 0.881165 0.675467 0.297099 0.032 Uiso 1 1 calc R . . . .
C37 C 0.9061(3) 0.59065(17) 0.24996(18) 0.0445(9) Uani 1 1 d . . . . .
H37A H 0.965812 0.562099 0.244212 0.067 Uiso 1 1 calc GR . . . .
H37B H 0.880682 0.606352 0.205468 0.067 Uiso 1 1 calc GR . . . .
H37C H 0.848648 0.568199 0.271411 0.067 Uiso 1 1 calc GR . . . .
C38 C 1.0322(3) 0.67986(15) 0.26122(17) 0.0364(8) Uani 1 1 d . . . . .
H38A H 1.056409 0.714893 0.290038 0.055 Uiso 1 1 calc GR . . . .
H38B H 1.006918 0.695887 0.216840 0.055 Uiso 1 1 calc GR . . . .
H38C H 1.091078 0.650756 0.255219 0.055 Uiso 1 1 calc GR . . . .
C39 C 0.9083(3) 0.66060(18) 0.55232(16) 0.0373(8) Uani 1 1 d . . . . .
H39 H 0.839127 0.679635 0.536788 0.045 Uiso 1 1 calc R . . . .
C40 C 0.8848(3) 0.61073(18) 0.60515(17) 0.0417(9) Uani 1 1 d . . . . .
H40A H 0.839661 0.578123 0.584166 0.063 Uiso 1 1 calc GR . . . .
H40B H 0.848287 0.630062 0.642702 0.063 Uiso 1 1 calc GR . . . .
H40C H 0.951466 0.591982 0.622477 0.063 Uiso 1 1 calc GR . . . .
C41 C 0.9762(3) 0.7126(2) 0.5839(2) 0.0586(11) Uani 1 1 d . . . . .
H41A H 1.045011 0.695452 0.599388 0.088 Uiso 1 1 calc GR . . . .
H41B H 0.940465 0.730431 0.622613 0.088 Uiso 1 1 calc GR . . . .
H41C H 0.986750 0.745362 0.550041 0.088 Uiso 1 1 calc GR . . . .
C42 C 0.4456(2) 0.75861(15) 0.54177(14) 0.0246(6) Uani 1 1 d . . . . .
C43 C 0.4634(3) 0.82416(15) 0.54578(15) 0.0327(8) Uani 1 1 d . . . . .
H43 H 0.533846 0.839711 0.549732 0.039 Uiso 1 1 calc R . . . .
C44 C 0.3788(3) 0.86591(19) 0.54400(17) 0.0455(10) Uani 1 1 d . . . . .
H44 H 0.392127 0.909705 0.546094 0.055 Uiso 1 1 calc R . . . .
C45 C 0.2764(3) 0.8446(2) 0.53925(18) 0.0525(11) Uani 1 1 d . . . . .
H45 H 0.219282 0.873599 0.538290 0.063 Uiso 1 1 calc R . . . .
C46 C 0.2560(3) 0.7817(2) 0.53588(17) 0.0519(12) Uani 1 1 d . . . . .
H46 H 0.184927 0.767117 0.532999 0.062 Uiso 1 1 calc R . . . .
C47 C 0.3407(3) 0.73846(18) 0.53669(15) 0.0363(8) Uani 1 1 d . . . . .
H47 H 0.325864 0.694880 0.533707 0.044 Uiso 1 1 calc R . . . .
C48 C 0.5170(3) 0.62399(15) 0.56214(18) 0.0402(9) Uani 1 1 d . . . . .
H48A H 0.470531 0.609267 0.524368 0.060 Uiso 1 1 calc GR . . . .
H48B H 0.477914 0.623910 0.604041 0.060 Uiso 1 1 calc GR . . . .
H48C H 0.578477 0.596136 0.567484 0.060 Uiso 1 1 calc GR . . . .
C49 C 0.6560(3) 0.73128(16) 0.61402(15) 0.0308(7) Uani 1 1 d . . . . .
H49A H 0.718680 0.704196 0.615920 0.046 Uiso 1 1 calc GR . . . .
H49B H 0.620935 0.729163 0.657377 0.046 Uiso 1 1 calc GR . . . .
H49C H 0.677444 0.774593 0.605396 0.046 Uiso 1 1 calc GR . . . .
C50 C 0.7844(2) 0.85459(13) 0.50874(14) 0.0231(6) Uani 1 1 d . . . . .
H50 H 0.859196 0.857759 0.515199 0.028 Uiso 1 1 calc R . . . .
C51 C 0.7744(2) 0.93526(13) 0.59042(15) 0.0250(6) Uani 1 1 d . . . . .
C52 C 0.8919(3) 0.92505(16) 0.60858(19) 0.0409(9) Uani 1 1 d . . . . .
H52A H 0.903306 0.881544 0.623057 0.061 Uiso 1 1 calc GR . . . .
H52B H 0.914269 0.953392 0.645576 0.061 Uiso 1 1 calc GR . . . .
H52C H 0.933428 0.933643 0.568753 0.061 Uiso 1 1 calc GR . . . .
C53 C 0.7102(3) 0.92804(17) 0.65428(17) 0.0454(10) Uani 1 1 d . . . . .
H53A H 0.634814 0.934220 0.642440 0.068 Uiso 1 1 calc GR . . . .
H53B H 0.733749 0.959353 0.688027 0.068 Uiso 1 1 calc GR . . . .
H53C H 0.721150 0.885934 0.673166 0.068 Uiso 1 1 calc GR . . . .
C54 C 0.7576(3) 1.00046(14) 0.56069(17) 0.0361(8) Uani 1 1 d . . . . .
H54A H 0.799889 1.005164 0.520455 0.054 Uiso 1 1 calc GR . . . .
H54B H 0.779631 1.031963 0.594604 0.054 Uiso 1 1 calc GR . . . .
H54C H 0.682419 1.006272 0.547854 0.054 Uiso 1 1 calc GR . . . .
N1 N 0.63063(17) 0.68902(10) 0.32874(11) 0.0163(5) Uani 1 1 d . . . . .
N2 N 0.75280(18) 0.80316(10) 0.32429(11) 0.0163(5) Uani 1 1 d . . . . .
N3 N 0.83775(18) 0.69208(10) 0.41376(11) 0.0189(5) Uani 1 1 d . . . . .
N4 N 0.72737(19) 0.89018(11) 0.54096(12) 0.0255(6) Uani 1 1 d . . . . .
O1 O 0.62280(15) 0.70575(9) 0.47208(9) 0.0204(4) Uani 1 1 d . . . . .
O2 O 0.74438(17) 0.81215(9) 0.46549(10) 0.0268(5) Uani 1 1 d . . . . .
Si Si 0.56232(6) 0.70444(4) 0.54429(4) 0.02088(18) Uani 1 1 d . . . . .
Nb Nb 0.72142(2) 0.73856(2) 0.40928(2) 0.01535(8) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.391(4) . ?
C1 C4 1.508(4) . ?
C1 N1 1.344(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.394(4) . ?
C3 C5 1.514(4) . ?
C3 N2 1.335(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.402(4) . ?
C6 C11 1.405(4) . ?
C6 N1 1.454(3) . ?
C7 C8 1.400(4) . ?
C7 C12 1.525(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.379(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.396(4) . ?
C11 C15 1.526(4) . ?
C12 H12 1.0000 . ?
C12 C13 1.533(4) . ?
C12 C14 1.532(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.530(4) . ?
C15 C17 1.519(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.405(4) . ?
C18 C23 1.405(4) . ?
C18 N2 1.455(3) . ?
C19 C20 1.397(4) . ?
C19 C24 1.527(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.391(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.366(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.398(4) . ?
C23 C27 1.517(4) . ?
C24 H24 1.0000 . ?
C24 C25 1.527(4) . ?
C24 C26 1.526(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27 1.0000 . ?
C27 C28 1.547(4) . ?
C27 C29 1.532(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.411(4) . ?
C30 C35 1.417(4) . ?
C30 N3 1.405(4) . ?
C31 C32 1.398(4) . ?
C31 C36 1.516(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.367(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.378(6) . ?
C34 H34 0.9500 . ?
C34 C35 1.392(5) . ?
C35 C39 1.517(5) . ?
C36 H36 1.0000 . ?
C36 C37 1.527(4) . ?
C36 C38 1.527(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39 1.0000 . ?
C39 C40 1.527(5) . ?
C39 C41 1.518(5) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.418(4) . ?
C42 C47 1.392(4) . ?
C42 Si 1.872(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.390(5) . ?
C44 H44 0.9500 . ?
C44 C45 1.371(6) . ?
C45 H45 0.9500 . ?
C45 C46 1.367(6) . ?
C46 H46 0.9500 . ?
C46 C47 1.412(5) . ?
C47 H47 0.9500 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C48 Si 1.848(3) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C49 Si 1.865(3) . ?
C50 H50 0.9500 . ?
C50 N4 1.240(4) . ?
C50 O2 1.329(3) . ?
C51 C52 1.526(4) . ?
C51 C53 1.534(4) . ?
C51 C54 1.521(4) . ?
C51 N4 1.476(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
N1 Nb 2.191(2) . ?
N2 Nb 2.218(2) . ?
N3 Nb 1.772(2) . ?
O1 Si 1.6441(19) . ?
O1 Nb 1.9247(18) . ?
O2 Nb 1.9366(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C4 116.3(2) . . ?
N1 C1 C2 123.9(3) . . ?
N1 C1 C4 119.8(2) . . ?
C1 C2 H2 116.0 . . ?
C1 C2 C3 127.9(3) . . ?
C3 C2 H2 116.0 . . ?
C2 C3 C5 115.7(2) . . ?
N2 C3 C2 123.6(2) . . ?
N2 C3 C5 120.7(2) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 121.5(3) . . ?
C7 C6 N1 119.7(3) . . ?
C11 C6 N1 118.7(2) . . ?
C6 C7 C12 123.0(2) . . ?
C8 C7 C6 117.6(3) . . ?
C8 C7 C12 119.4(3) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 C7 121.5(3) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.2(3) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.6(3) . . ?
C11 C10 H10 119.7 . . ?
C6 C11 C15 122.2(2) . . ?
C10 C11 C6 118.6(3) . . ?
C10 C11 C15 119.1(3) . . ?
C7 C12 H12 108.0 . . ?
C7 C12 C13 112.1(3) . . ?
C7 C12 C14 111.3(2) . . ?
C13 C12 H12 108.0 . . ?
C14 C12 H12 108.0 . . ?
C14 C12 C13 109.4(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15 108.2 . . ?
C11 C15 C16 111.3(3) . . ?
C16 C15 H15 108.2 . . ?
C17 C15 C11 112.8(2) . . ?
C17 C15 H15 108.2 . . ?
C17 C15 C16 108.1(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 122.2(3) . . ?
C19 C18 N2 117.7(2) . . ?
C23 C18 N2 120.1(2) . . ?
C18 C19 C24 122.0(2) . . ?
C20 C19 C18 117.3(3) . . ?
C20 C19 C24 120.7(3) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 C19 121.3(3) . . ?
C21 C20 H20 119.4 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.0(3) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 119.2 . . ?
C21 C22 C23 121.6(3) . . ?
C23 C22 H22 119.2 . . ?
C18 C23 C27 123.5(2) . . ?
C22 C23 C18 117.5(3) . . ?
C22 C23 C27 118.9(3) . . ?
C19 C24 H24 107.1 . . ?
C19 C24 C25 112.7(2) . . ?
C25 C24 H24 107.1 . . ?
C26 C24 C19 111.7(2) . . ?
C26 C24 H24 107.1 . . ?
C26 C24 C25 110.9(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27 107.7 . . ?
C23 C27 C28 112.5(3) . . ?
C23 C27 C29 111.1(2) . . ?
C28 C27 H27 107.7 . . ?
C29 C27 H27 107.7 . . ?
C29 C27 C28 110.1(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C35 120.5(3) . . ?
N3 C30 C31 119.5(3) . . ?
N3 C30 C35 120.0(3) . . ?
C30 C31 C36 122.2(3) . . ?
C32 C31 C30 118.2(3) . . ?
C32 C31 C36 119.6(3) . . ?
C31 C32 H32 119.2 . . ?
C33 C32 C31 121.6(3) . . ?
C33 C32 H32 119.2 . . ?
C32 C33 H33 119.9 . . ?
C32 C33 C34 120.1(3) . . ?
C34 C33 H33 119.9 . . ?
C33 C34 H34 119.3 . . ?
C33 C34 C35 121.4(3) . . ?
C35 C34 H34 119.3 . . ?
C30 C35 C39 121.6(3) . . ?
C34 C35 C30 118.2(3) . . ?
C34 C35 C39 120.2(3) . . ?
C31 C36 H36 107.7 . . ?
C31 C36 C37 113.3(3) . . ?
C31 C36 C38 111.1(3) . . ?
C37 C36 H36 107.7 . . ?
C38 C36 H36 107.7 . . ?
C38 C36 C37 109.0(3) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C39 H39 107.4 . . ?
C35 C39 C40 112.8(3) . . ?
C35 C39 C41 111.0(3) . . ?
C40 C39 H39 107.4 . . ?
C41 C39 H39 107.4 . . ?
C41 C39 C40 110.6(3) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 Si 119.0(2) . . ?
C47 C42 C43 117.1(3) . . ?
C47 C42 Si 123.8(3) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 C42 120.7(3) . . ?
C44 C43 H43 119.6 . . ?
C43 C44 H44 119.6 . . ?
C45 C44 C43 120.7(4) . . ?
C45 C44 H44 119.6 . . ?
C44 C45 H45 119.9 . . ?
C46 C45 C44 120.3(4) . . ?
C46 C45 H45 119.9 . . ?
C45 C46 H46 120.0 . . ?
C45 C46 C47 120.0(4) . . ?
C47 C46 H46 120.0 . . ?
C42 C47 C46 121.1(4) . . ?
C42 C47 H47 119.4 . . ?
C46 C47 H47 119.4 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
Si C48 H48A 109.5 . . ?
Si C48 H48B 109.5 . . ?
Si C48 H48C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
Si C49 H49A 109.5 . . ?
Si C49 H49B 109.5 . . ?
Si C49 H49C 109.5 . . ?
N4 C50 H50 118.9 . . ?
N4 C50 O2 122.2(3) . . ?
O2 C50 H50 118.9 . . ?
C52 C51 C53 109.6(3) . . ?
C54 C51 C52 109.9(3) . . ?
C54 C51 C53 109.8(3) . . ?
N4 C51 C52 115.0(3) . . ?
N4 C51 C53 105.3(2) . . ?
N4 C51 C54 107.2(2) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C1 N1 C6 116.1(2) . . ?
C1 N1 Nb 125.87(18) . . ?
C6 N1 Nb 117.75(16) . . ?
C3 N2 C18 116.3(2) . . ?
C3 N2 Nb 126.27(18) . . ?
C18 N2 Nb 117.02(16) . . ?
C30 N3 Nb 172.9(2) . . ?
C50 N4 C51 120.7(3) . . ?
Si O1 Nb 154.18(12) . . ?
C50 O2 Nb 164.4(2) . . ?
C48 Si C42 109.19(16) . . ?
C48 Si C49 109.68(16) . . ?
C49 Si C42 107.68(14) . . ?
O1 Si C42 111.14(11) . . ?
O1 Si C48 109.86(13) . . ?
O1 Si C49 109.25(13) . . ?
N1 Nb N2 81.79(8) . . ?
N3 Nb N1 99.99(9) . . ?
N3 Nb N2 102.19(9) . . ?
N3 Nb O1 108.80(9) . . ?
N3 Nb O2 108.76(10) . . ?
O1 Nb N1 87.57(8) . . ?
O1 Nb N2 148.55(8) . . ?
O1 Nb O2 90.69(8) . . ?
O2 Nb N1 150.12(9) . . ?
O2 Nb N2 84.33(8) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bmkxr44
_database_code_depnum_ccdc_archive 'CCDC 2004316'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-17 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_audit_creation_date             2020-05-17
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            (κ1-BDI)Nb(NtBu)(NHtBu)(SCPh3)
_chemical_name_systematic        
(tert-butyl)amino-(tert-butyl)imino-(triphenylmethylthiolato)-(N-(4-((2,6-diisopropylphenyl)imino)pent-2-en-2-yl)-2,6-diisopropylanilido)-niobium(V)
_chemical_formula_moiety         'C56 H75 N4 Nb S'
_chemical_formula_sum            'C56 H75 N4 Nb S'
_chemical_formula_weight         929.17
_chemical_melting_point          442
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.4066(4)
_cell_length_b                   13.5108(4)
_cell_length_c                   14.4569(4)
_cell_angle_alpha                101.7150(10)
_cell_angle_beta                 96.702(2)
_cell_angle_gamma                90.848(2)
_cell_volume                     2544.57(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.91
_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.975
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0897 before and 0.0529 after correction.
The Ratio of minimum to maximum transmission is 0.9457.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            57967
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.426
_diffrn_reflns_theta_min         1.449
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8059
_reflns_number_total             9328
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         9328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0329
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0289P)²+2.0561P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0799
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C40(H40),
 C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49),
  C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), N4(H4)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.20463(15) 0.36415(14) 0.81618(14) 0.0165(4) Uani 1 1 d . . . . .
C2 C 0.12425(15) 0.40876(14) 0.77878(15) 0.0180(4) Uani 1 1 d . . . . .
H2 H 0.062162 0.396694 0.801016 0.022 Uiso 1 1 calc R . . . .
C3 C 0.12071(15) 0.47328(14) 0.70837(15) 0.0167(4) Uani 1 1 d . . . . .
C4 C 0.30952(15) 0.37708(15) 0.79189(16) 0.0200(5) Uani 1 1 d . . . . .
H4A H 0.306574 0.401559 0.732328 0.030 Uiso 1 1 calc GR . . . .
H4B H 0.342022 0.311909 0.784312 0.030 Uiso 1 1 calc GR . . . .
H4C H 0.348286 0.426180 0.843195 0.030 Uiso 1 1 calc GR . . . .
C5 C 0.02365(16) 0.46312(16) 0.64158(16) 0.0251(5) Uani 1 1 d . . . . .
H5A H 0.016561 0.523263 0.613552 0.038 Uiso 1 1 calc GR . . . .
H5B H -0.033230 0.456620 0.677084 0.038 Uiso 1 1 calc GR . . . .
H5C H 0.024787 0.402909 0.590862 0.038 Uiso 1 1 calc GR . . . .
C6 C 0.10436(15) 0.29105(15) 0.91858(16) 0.0198(5) Uani 1 1 d . . . . .
C7 C 0.09634(17) 0.34419(16) 1.01204(16) 0.0248(5) Uani 1 1 d . . . . .
C8 C 0.00766(19) 0.33106(19) 1.0501(2) 0.0351(6) Uani 1 1 d . . . . .
H8 H 0.000785 0.365856 1.112978 0.042 Uiso 1 1 calc R . . . .
C9 C -0.07041(19) 0.2687(2) 0.9987(2) 0.0393(7) Uani 1 1 d . . . . .
H9 H -0.130239 0.260819 1.026203 0.047 Uiso 1 1 calc R . . . .
C10 C -0.06200(17) 0.21760(18) 0.9073(2) 0.0332(6) Uani 1 1 d . . . . .
H10 H -0.116318 0.174653 0.872647 0.040 Uiso 1 1 calc R . . . .
C11 C 0.02526(16) 0.22786(16) 0.86464(17) 0.0235(5) Uani 1 1 d . . . . .
C12 C 0.18118(18) 0.41389(17) 1.06952(16) 0.0285(5) Uani 1 1 d . . . . .
H12 H 0.245869 0.381715 1.055273 0.034 Uiso 1 1 calc R . . . .
C13 C 0.1816(2) 0.51570(19) 1.03976(19) 0.0434(7) Uani 1 1 d . . . . .
H13A H 0.186609 0.505228 0.971393 0.065 Uiso 1 1 calc GR . . . .
H13B H 0.239210 0.557901 1.075220 0.065 Uiso 1 1 calc GR . . . .
H13C H 0.119229 0.549504 1.053509 0.065 Uiso 1 1 calc GR . . . .
C14 C 0.1802(2) 0.4335(2) 1.17706(18) 0.0449(7) Uani 1 1 d . . . . .
H14A H 0.123653 0.475602 1.194392 0.067 Uiso 1 1 calc GR . . . .
H14B H 0.243322 0.468538 1.208832 0.067 Uiso 1 1 calc GR . . . .
H14C H 0.172995 0.368932 1.197079 0.067 Uiso 1 1 calc GR . . . .
C15 C 0.03151(17) 0.17149(16) 0.76380(17) 0.0266(5) Uani 1 1 d . . . . .
H15 H 0.094307 0.196175 0.743146 0.032 Uiso 1 1 calc R . . . .
C16 C -0.0572(2) 0.19306(19) 0.6951(2) 0.0416(7) Uani 1 1 d . . . . .
H16A H -0.119684 0.166990 0.712083 0.062 Uiso 1 1 calc GR . . . .
H16B H -0.048097 0.159816 0.629986 0.062 Uiso 1 1 calc GR . . . .
H16C H -0.060638 0.266218 0.699326 0.062 Uiso 1 1 calc GR . . . .
C17 C 0.03857(19) 0.05765(17) 0.75773(19) 0.0327(6) Uani 1 1 d . . . . .
H17A H 0.097149 0.044633 0.800225 0.049 Uiso 1 1 calc GR . . . .
H17B H 0.045618 0.024122 0.692168 0.049 Uiso 1 1 calc GR . . . .
H17C H -0.022524 0.031172 0.776913 0.049 Uiso 1 1 calc GR . . . .
C18 C 0.18879(15) 0.59097(15) 0.63162(15) 0.0182(4) Uani 1 1 d . . . . .
C19 C 0.14985(15) 0.68823(15) 0.64945(16) 0.0213(5) Uani 1 1 d . . . . .
C20 C 0.15332(16) 0.74632(16) 0.57937(17) 0.0252(5) Uani 1 1 d . . . . .
H20 H 0.127526 0.812251 0.589547 0.030 Uiso 1 1 calc R . . . .
C21 C 0.19352(17) 0.70934(17) 0.49605(17) 0.0274(5) Uani 1 1 d . . . . .
H21 H 0.196638 0.750306 0.450185 0.033 Uiso 1 1 calc R . . . .
C22 C 0.22913(17) 0.61290(16) 0.47944(16) 0.0246(5) Uani 1 1 d . . . . .
H22 H 0.255449 0.587587 0.421370 0.029 Uiso 1 1 calc R . . . .
C23 C 0.22723(15) 0.55192(15) 0.54623(15) 0.0201(5) Uani 1 1 d . . . . .
C24 C 0.26997(16) 0.44784(16) 0.52945(16) 0.0230(5) Uani 1 1 d . . . . .
H24 H 0.235900 0.406958 0.567936 0.028 Uiso 1 1 calc R . . . .
C25 C 0.2514(2) 0.39188(19) 0.42505(18) 0.0396(6) Uani 1 1 d . . . . .
H25A H 0.180480 0.395464 0.400822 0.059 Uiso 1 1 calc GR . . . .
H25B H 0.268505 0.320914 0.420478 0.059 Uiso 1 1 calc GR . . . .
H25C H 0.293484 0.423530 0.387177 0.059 Uiso 1 1 calc GR . . . .
C26 C 0.38219(17) 0.45480(18) 0.56515(18) 0.0303(5) Uani 1 1 d . . . . .
H26A H 0.417851 0.493486 0.527815 0.045 Uiso 1 1 calc GR . . . .
H26B H 0.408095 0.386569 0.558145 0.045 Uiso 1 1 calc GR . . . .
H26C H 0.392625 0.488802 0.632379 0.045 Uiso 1 1 calc GR . . . .
C27 C 0.10662(17) 0.73116(16) 0.74071(17) 0.0263(5) Uani 1 1 d . . . . .
H27 H 0.103398 0.675842 0.777043 0.032 Uiso 1 1 calc R . . . .
C28 C 0.00060(18) 0.76740(19) 0.7228(2) 0.0397(6) Uani 1 1 d . . . . .
H28A H 0.001661 0.822726 0.688331 0.060 Uiso 1 1 calc GR . . . .
H28B H -0.025169 0.791469 0.783808 0.060 Uiso 1 1 calc GR . . . .
H28C H -0.043020 0.711343 0.684802 0.060 Uiso 1 1 calc GR . . . .
C29 C 0.17389(18) 0.81751(19) 0.80316(18) 0.0345(6) Uani 1 1 d . . . . .
H29A H 0.240656 0.792561 0.819127 0.052 Uiso 1 1 calc GR . . . .
H29B H 0.144167 0.843085 0.861785 0.052 Uiso 1 1 calc GR . . . .
H29C H 0.179942 0.872213 0.768582 0.052 Uiso 1 1 calc GR . . . .
C30 C 0.24025(16) 0.08826(16) 1.05872(16) 0.0232(5) Uani 1 1 d . . . . .
C31 C 0.30139(19) -0.00728(18) 1.0468(2) 0.0367(6) Uani 1 1 d . . . . .
H31A H 0.293040 -0.041750 0.979695 0.055 Uiso 1 1 calc GR . . . .
H31B H 0.277701 -0.052578 1.085375 0.055 Uiso 1 1 calc GR . . . .
H31C H 0.372597 0.011294 1.067727 0.055 Uiso 1 1 calc GR . . . .
C32 C 0.12884(17) 0.06052(18) 1.02515(18) 0.0295(5) Uani 1 1 d . . . . .
H32A H 0.091189 0.122456 1.027897 0.044 Uiso 1 1 calc GR . . . .
H32B H 0.102725 0.019790 1.066546 0.044 Uiso 1 1 calc GR . . . .
H32C H 0.121347 0.021554 0.959538 0.044 Uiso 1 1 calc GR . . . .
C33 C 0.2530(2) 0.1456(2) 1.16174(17) 0.0382(6) Uani 1 1 d . . . . .
H33A H 0.324226 0.164064 1.182503 0.057 Uiso 1 1 calc GR . . . .
H33B H 0.228621 0.102602 1.202076 0.057 Uiso 1 1 calc GR . . . .
H33C H 0.214282 0.207038 1.166992 0.057 Uiso 1 1 calc GR . . . .
C34 C 0.51069(16) 0.30956(17) 1.06732(16) 0.0261(5) Uani 1 1 d . . . . .
C35 C 0.60990(19) 0.3575(2) 1.05277(19) 0.0416(7) Uani 1 1 d . . . . .
H35A H 0.642687 0.310153 1.006049 0.062 Uiso 1 1 calc GR . . . .
H35B H 0.653824 0.373141 1.113403 0.062 Uiso 1 1 calc GR . . . .
H35C H 0.596920 0.419891 1.029517 0.062 Uiso 1 1 calc GR . . . .
C36 C 0.4630(2) 0.3776(2) 1.14543(18) 0.0430(7) Uani 1 1 d . . . . .
H36A H 0.449375 0.442678 1.127494 0.065 Uiso 1 1 calc GR . . . .
H36B H 0.508951 0.388635 1.204820 0.065 Uiso 1 1 calc GR . . . .
H36C H 0.399881 0.345479 1.154542 0.065 Uiso 1 1 calc GR . . . .
C37 C 0.52989(19) 0.20677(19) 1.09248(18) 0.0361(6) Uani 1 1 d . . . . .
H37A H 0.466005 0.174755 1.099785 0.054 Uiso 1 1 calc GR . . . .
H37B H 0.574920 0.215693 1.152288 0.054 Uiso 1 1 calc GR . . . .
H37C H 0.561078 0.163735 1.041540 0.054 Uiso 1 1 calc GR . . . .
C38 C 0.39871(15) 0.05700(15) 0.69233(15) 0.0175(4) Uani 1 1 d . . . . .
C39 C 0.31494(16) 0.06495(15) 0.61174(15) 0.0206(5) Uani 1 1 d . . . . .
C40 C 0.24619(17) 0.14030(17) 0.62355(17) 0.0281(5) Uani 1 1 d . . . . .
H40 H 0.248707 0.185498 0.683483 0.034 Uiso 1 1 calc R . . . .
C41 C 0.17356(18) 0.15176(19) 0.55024(18) 0.0352(6) Uani 1 1 d . . . . .
H41 H 0.127803 0.204823 0.560007 0.042 Uiso 1 1 calc R . . . .
C42 C 0.16793(18) 0.08587(19) 0.46304(18) 0.0353(6) Uani 1 1 d . . . . .
H42 H 0.117741 0.092624 0.412841 0.042 Uiso 1 1 calc R . . . .
C43 C 0.23558(18) 0.01052(18) 0.44964(17) 0.0323(6) Uani 1 1 d . . . . .
H43 H 0.232257 -0.034687 0.389639 0.039 Uiso 1 1 calc R . . . .
C44 C 0.30904(17) -0.00041(17) 0.52298(16) 0.0257(5) Uani 1 1 d . . . . .
H44 H 0.355468 -0.052776 0.512496 0.031 Uiso 1 1 calc R . . . .
C45 C 0.44446(16) -0.04798(15) 0.67192(14) 0.0191(4) Uani 1 1 d . . . . .
C46 C 0.38390(17) -0.13371(15) 0.66865(16) 0.0234(5) Uani 1 1 d . . . . .
H46 H 0.316269 -0.125836 0.681548 0.028 Uiso 1 1 calc R . . . .
C47 C 0.42009(17) -0.23000(16) 0.64704(16) 0.0253(5) Uani 1 1 d . . . . .
H47 H 0.377512 -0.287329 0.645378 0.030 Uiso 1 1 calc R . . . .
C48 C 0.51789(17) -0.24266(16) 0.62795(16) 0.0263(5) Uani 1 1 d . . . . .
H48 H 0.543227 -0.308618 0.613816 0.032 Uiso 1 1 calc R . . . .
C49 C 0.57887(17) -0.15911(17) 0.62944(16) 0.0262(5) Uani 1 1 d . . . . .
H49 H 0.646091 -0.167688 0.615476 0.031 Uiso 1 1 calc R . . . .
C50 C 0.54230(16) -0.06188(16) 0.65140(15) 0.0220(5) Uani 1 1 d . . . . .
H50 H 0.584908 -0.004810 0.652261 0.026 Uiso 1 1 calc R . . . .
C51 C 0.48090(15) 0.14032(15) 0.70397(15) 0.0183(4) Uani 1 1 d . . . . .
C52 C 0.55251(15) 0.16009(15) 0.78480(15) 0.0206(5) Uani 1 1 d . . . . .
H52 H 0.545288 0.127580 0.836201 0.025 Uiso 1 1 calc R . . . .
C53 C 0.63356(16) 0.22640(17) 0.79055(17) 0.0267(5) Uani 1 1 d . . . . .
H53 H 0.681565 0.238822 0.845785 0.032 Uiso 1 1 calc R . . . .
C54 C 0.64555(17) 0.27489(17) 0.71677(17) 0.0288(5) Uani 1 1 d . . . . .
H54 H 0.701572 0.320156 0.720959 0.035 Uiso 1 1 calc R . . . .
C55 C 0.57510(17) 0.25673(17) 0.63694(18) 0.0302(5) Uani 1 1 d . . . . .
H55 H 0.582464 0.290160 0.586178 0.036 Uiso 1 1 calc R . . . .
C56 C 0.49356(16) 0.18993(16) 0.63032(16) 0.0240(5) Uani 1 1 d . . . . .
H56 H 0.445849 0.177929 0.574875 0.029 Uiso 1 1 calc R . . . .
N1 N 0.19807(12) 0.29943(12) 0.87964(12) 0.0157(4) Uani 1 1 d . . . . .
N2 N 0.19490(12) 0.53287(12) 0.70452(12) 0.0181(4) Uani 1 1 d . . . . .
N3 N 0.27691(13) 0.15275(12) 0.99878(12) 0.0186(4) Uani 1 1 d . . . . .
N4 N 0.44183(13) 0.29440(13) 0.97694(12) 0.0204(4) Uani 1 1 d . . . . .
H4 H 0.462281 0.332488 0.939610 0.024 Uiso 1 1 calc R . . . .
S1 S 0.34126(4) 0.05881(4) 0.80552(4) 0.01887(12) Uani 1 1 d . . . . .
Nb1 Nb 0.31864(2) 0.21520(2) 0.91483(2) 0.01563(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.354(3) . ?
C1 C4 1.505(3) . ?
C1 N1 1.399(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.466(3) . ?
C3 C5 1.514(3) . ?
C3 N2 1.284(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.413(3) . ?
C6 C11 1.404(3) . ?
C6 N1 1.447(3) . ?
C7 C8 1.391(3) . ?
C7 C12 1.517(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.377(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.378(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.403(3) . ?
C11 C15 1.514(3) . ?
C12 H12 1.0000 . ?
C12 C13 1.522(3) . ?
C12 C14 1.525(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.529(3) . ?
C15 C17 1.528(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.407(3) . ?
C18 C23 1.400(3) . ?
C18 N2 1.432(3) . ?
C19 C20 1.406(3) . ?
C19 C27 1.513(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.381(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.379(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.393(3) . ?
C23 C24 1.511(3) . ?
C24 H24 1.0000 . ?
C24 C25 1.535(3) . ?
C24 C26 1.528(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27 1.0000 . ?
C27 C28 1.521(3) . ?
C27 C29 1.530(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.530(3) . ?
C30 C32 1.532(3) . ?
C30 C33 1.522(3) . ?
C30 N3 1.465(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.526(3) . ?
C34 C36 1.514(3) . ?
C34 C37 1.524(3) . ?
C34 N4 1.485(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.543(3) . ?
C38 C45 1.540(3) . ?
C38 C51 1.534(3) . ?
C38 S1 1.884(2) . ?
C39 C40 1.382(3) . ?
C39 C44 1.395(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.388(3) . ?
C41 H41 0.9500 . ?
C41 C42 1.381(4) . ?
C42 H42 0.9500 . ?
C42 C43 1.373(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.393(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.394(3) . ?
C45 C50 1.385(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.384(3) . ?
C47 H47 0.9500 . ?
C47 C48 1.377(3) . ?
C48 H48 0.9500 . ?
C48 C49 1.379(3) . ?
C49 H49 0.9500 . ?
C49 C50 1.397(3) . ?
C50 H50 0.9500 . ?
C51 C52 1.401(3) . ?
C51 C56 1.393(3) . ?
C52 H52 0.9500 . ?
C52 C53 1.382(3) . ?
C53 H53 0.9500 . ?
C53 C54 1.383(3) . ?
C54 H54 0.9500 . ?
C54 C55 1.381(3) . ?
C55 H55 0.9500 . ?
C55 C56 1.389(3) . ?
C56 H56 0.9500 . ?
N1 Nb1 2.0651(16) . ?
N3 Nb1 1.7486(17) . ?
N4 H4 0.8800 . ?
N4 Nb1 1.9724(17) . ?
S1 Nb1 2.4143(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C4 123.47(18) . . ?
C2 C1 N1 123.31(18) . . ?
N1 C1 C4 113.20(16) . . ?
C1 C2 H2 115.8 . . ?
C1 C2 C3 128.32(19) . . ?
C3 C2 H2 115.8 . . ?
C2 C3 C5 114.61(17) . . ?
N2 C3 C2 121.85(18) . . ?
N2 C3 C5 123.54(18) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 118.70(19) . . ?
C11 C6 C7 121.5(2) . . ?
C11 C6 N1 119.72(19) . . ?
C6 C7 C12 121.4(2) . . ?
C8 C7 C6 117.9(2) . . ?
C8 C7 C12 120.7(2) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 C7 121.4(2) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120.2(2) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 119.4 . . ?
C9 C10 C11 121.2(2) . . ?
C11 C10 H10 119.4 . . ?
C6 C11 C15 122.47(19) . . ?
C10 C11 C6 117.7(2) . . ?
C10 C11 C15 119.8(2) . . ?
C7 C12 H12 107.5 . . ?
C7 C12 C13 111.00(19) . . ?
C7 C12 C14 114.9(2) . . ?
C13 C12 H12 107.5 . . ?
C13 C12 C14 108.0(2) . . ?
C14 C12 H12 107.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15 107.7 . . ?
C11 C15 C16 111.6(2) . . ?
C11 C15 C17 111.79(19) . . ?
C16 C15 H15 107.7 . . ?
C17 C15 H15 107.7 . . ?
C17 C15 C16 110.22(19) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N2 119.37(19) . . ?
C23 C18 C19 121.47(19) . . ?
C23 C18 N2 119.05(18) . . ?
C18 C19 C27 122.24(19) . . ?
C20 C19 C18 117.6(2) . . ?
C20 C19 C27 120.15(19) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 C19 121.2(2) . . ?
C21 C20 H20 119.4 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.0(2) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 119.4 . . ?
C21 C22 C23 121.2(2) . . ?
C23 C22 H22 119.4 . . ?
C18 C23 C24 120.41(19) . . ?
C22 C23 C18 118.46(19) . . ?
C22 C23 C24 121.1(2) . . ?
C23 C24 H24 107.6 . . ?
C23 C24 C25 113.22(18) . . ?
C23 C24 C26 110.15(18) . . ?
C25 C24 H24 107.6 . . ?
C26 C24 H24 107.6 . . ?
C26 C24 C25 110.44(19) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 C27 H27 107.7 . . ?
C19 C27 C28 112.6(2) . . ?
C19 C27 C29 111.56(19) . . ?
C28 C27 H27 107.7 . . ?
C28 C27 C29 109.52(19) . . ?
C29 C27 H27 107.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C32 110.07(19) . . ?
C33 C30 C31 111.3(2) . . ?
C33 C30 C32 109.8(2) . . ?
N3 C30 C31 107.59(18) . . ?
N3 C30 C32 108.76(17) . . ?
N3 C30 C33 109.26(18) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C36 C34 C35 110.4(2) . . ?
C36 C34 C37 110.4(2) . . ?
C37 C34 C35 109.2(2) . . ?
N4 C34 C35 108.79(19) . . ?
N4 C34 C36 109.43(18) . . ?
N4 C34 C37 108.60(18) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 S1 109.23(14) . . ?
C45 C38 C39 109.84(16) . . ?
C45 C38 S1 103.49(13) . . ?
C51 C38 C39 111.34(16) . . ?
C51 C38 C45 110.20(16) . . ?
C51 C38 S1 112.45(14) . . ?
C40 C39 C38 121.02(19) . . ?
C40 C39 C44 117.7(2) . . ?
C44 C39 C38 121.19(19) . . ?
C39 C40 H40 119.1 . . ?
C39 C40 C41 121.8(2) . . ?
C41 C40 H40 119.1 . . ?
C40 C41 H41 120.1 . . ?
C42 C41 C40 119.9(2) . . ?
C42 C41 H41 120.1 . . ?
C41 C42 H42 120.3 . . ?
C43 C42 C41 119.3(2) . . ?
C43 C42 H42 120.3 . . ?
C42 C43 H43 119.6 . . ?
C42 C43 C44 120.8(2) . . ?
C44 C43 H43 119.6 . . ?
C39 C44 H44 119.7 . . ?
C43 C44 C39 120.5(2) . . ?
C43 C44 H44 119.7 . . ?
C46 C45 C38 119.10(18) . . ?
C50 C45 C38 122.85(18) . . ?
C50 C45 C46 117.95(19) . . ?
C45 C46 H46 119.3 . . ?
C47 C46 C45 121.5(2) . . ?
C47 C46 H46 119.3 . . ?
C46 C47 H47 120.0 . . ?
C48 C47 C46 119.9(2) . . ?
C48 C47 H47 120.0 . . ?
C47 C48 H48 120.2 . . ?
C47 C48 C49 119.7(2) . . ?
C49 C48 H48 120.2 . . ?
C48 C49 H49 119.8 . . ?
C48 C49 C50 120.3(2) . . ?
C50 C49 H49 119.8 . . ?
C45 C50 C49 120.6(2) . . ?
C45 C50 H50 119.7 . . ?
C49 C50 H50 119.7 . . ?
C52 C51 C38 120.47(19) . . ?
C56 C51 C38 121.07(18) . . ?
C56 C51 C52 118.04(19) . . ?
C51 C52 H52 119.7 . . ?
C53 C52 C51 120.7(2) . . ?
C53 C52 H52 119.7 . . ?
C52 C53 H53 119.6 . . ?
C52 C53 C54 120.7(2) . . ?
C54 C53 H53 119.6 . . ?
C53 C54 H54 120.4 . . ?
C55 C54 C53 119.2(2) . . ?
C55 C54 H54 120.4 . . ?
C54 C55 H55 119.8 . . ?
C54 C55 C56 120.5(2) . . ?
C56 C55 H55 119.8 . . ?
C51 C56 H56 119.6 . . ?
C55 C56 C51 120.8(2) . . ?
C55 C56 H56 119.6 . . ?
C1 N1 C6 118.66(15) . . ?
C1 N1 Nb1 120.68(13) . . ?
C6 N1 Nb1 120.66(12) . . ?
C3 N2 C18 119.36(17) . . ?
C30 N3 Nb1 172.25(15) . . ?
C34 N4 H4 110.2 . . ?
C34 N4 Nb1 139.51(15) . . ?
Nb1 N4 H4 110.2 . . ?
C38 S1 Nb1 121.63(6) . . ?
N1 Nb1 S1 117.21(5) . . ?
N3 Nb1 N1 103.71(7) . . ?
N3 Nb1 N4 106.73(8) . . ?
N3 Nb1 S1 92.92(6) . . ?
N4 Nb1 N1 115.29(7) . . ?
N4 Nb1 S1 116.58(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C5 146.7(2) . . . . ?
C1 C2 C3 N2 -33.1(3) . . . . ?
C2 C1 N1 C6 -9.5(3) . . . . ?
C2 C1 N1 Nb1 169.17(15) . . . . ?
C2 C3 N2 C18 177.37(18) . . . . ?
C4 C1 C2 C3 1.9(3) . . . . ?
C4 C1 N1 C6 171.90(17) . . . . ?
C4 C1 N1 Nb1 -9.4(2) . . . . ?
C5 C3 N2 C18 -2.4(3) . . . . ?
C6 C7 C8 C9 -0.3(3) . . . . ?
C6 C7 C12 C13 79.4(3) . . . . ?
C6 C7 C12 C14 -157.7(2) . . . . ?
C6 C11 C15 C16 -126.2(2) . . . . ?
C6 C11 C15 C17 109.8(2) . . . . ?
C7 C6 C11 C10 -1.1(3) . . . . ?
C7 C6 C11 C15 179.00(18) . . . . ?
C7 C6 N1 C1 -101.3(2) . . . . ?
C7 C6 N1 Nb1 80.0(2) . . . . ?
C7 C8 C9 C10 -0.1(4) . . . . ?
C8 C7 C12 C13 -100.4(3) . . . . ?
C8 C7 C12 C14 22.6(3) . . . . ?
C8 C9 C10 C11 -0.2(3) . . . . ?
C9 C10 C11 C6 0.8(3) . . . . ?
C9 C10 C11 C15 -179.4(2) . . . . ?
C10 C11 C15 C16 53.9(3) . . . . ?
C10 C11 C15 C17 -70.1(2) . . . . ?
C11 C6 C7 C8 0.9(3) . . . . ?
C11 C6 C7 C12 -178.88(18) . . . . ?
C11 C6 N1 C1 81.1(2) . . . . ?
C11 C6 N1 Nb1 -97.58(19) . . . . ?
C12 C7 C8 C9 179.5(2) . . . . ?
C18 C19 C20 C21 0.0(3) . . . . ?
C18 C19 C27 C28 -126.0(2) . . . . ?
C18 C19 C27 C29 110.4(2) . . . . ?
C18 C23 C24 C25 146.1(2) . . . . ?
C18 C23 C24 C26 -89.7(2) . . . . ?
C19 C18 C23 C22 1.9(3) . . . . ?
C19 C18 C23 C24 179.12(19) . . . . ?
C19 C18 N2 C3 90.7(2) . . . . ?
C19 C20 C21 C22 1.5(3) . . . . ?
C20 C19 C27 C28 54.8(3) . . . . ?
C20 C19 C27 C29 -68.8(3) . . . . ?
C20 C21 C22 C23 -1.2(3) . . . . ?
C21 C22 C23 C18 -0.4(3) . . . . ?
C21 C22 C23 C24 -177.6(2) . . . . ?
C22 C23 C24 C25 -36.8(3) . . . . ?
C22 C23 C24 C26 87.4(2) . . . . ?
C23 C18 C19 C20 -1.7(3) . . . . ?
C23 C18 C19 C27 179.11(19) . . . . ?
C23 C18 N2 C3 -93.0(2) . . . . ?
C27 C19 C20 C21 179.2(2) . . . . ?
C35 C34 N4 Nb1 161.62(18) . . . . ?
C36 C34 N4 Nb1 -77.7(3) . . . . ?
C37 C34 N4 Nb1 42.8(3) . . . . ?
C38 C39 C40 C41 176.6(2) . . . . ?
C38 C39 C44 C43 -177.2(2) . . . . ?
C38 C45 C46 C47 177.51(19) . . . . ?
C38 C45 C50 C49 -177.28(19) . . . . ?
C38 C51 C52 C53 172.23(19) . . . . ?
C38 C51 C56 C55 -172.4(2) . . . . ?
C39 C38 C45 C46 -63.5(2) . . . . ?
C39 C38 C45 C50 112.9(2) . . . . ?
C39 C38 C51 C52 166.66(18) . . . . ?
C39 C38 C51 C56 -20.9(3) . . . . ?
C39 C38 S1 Nb1 -89.30(13) . . . . ?
C39 C40 C41 C42 0.9(4) . . . . ?
C40 C39 C44 C43 -0.3(3) . . . . ?
C40 C41 C42 C43 -1.0(4) . . . . ?
C41 C42 C43 C44 0.4(4) . . . . ?
C42 C43 C44 C39 0.3(4) . . . . ?
C44 C39 C40 C41 -0.2(3) . . . . ?
C45 C38 C39 C40 164.1(2) . . . . ?
C45 C38 C39 C44 -19.2(3) . . . . ?
C45 C38 C51 C52 -71.2(2) . . . . ?
C45 C38 C51 C56 101.3(2) . . . . ?
C45 C38 S1 Nb1 153.74(10) . . . . ?
C45 C46 C47 C48 -0.2(3) . . . . ?
C46 C45 C50 C49 -0.9(3) . . . . ?
C46 C47 C48 C49 -0.7(3) . . . . ?
C47 C48 C49 C50 0.8(3) . . . . ?
C48 C49 C50 C45 0.0(3) . . . . ?
C50 C45 C46 C47 0.9(3) . . . . ?
C51 C38 C39 C40 -73.6(3) . . . . ?
C51 C38 C39 C44 103.2(2) . . . . ?
C51 C38 C45 C46 173.52(19) . . . . ?
C51 C38 C45 C50 -10.1(3) . . . . ?
C51 C38 S1 Nb1 34.84(16) . . . . ?
C51 C52 C53 C54 0.2(3) . . . . ?
C52 C51 C56 C55 0.2(3) . . . . ?
C52 C53 C54 C55 0.3(3) . . . . ?
C53 C54 C55 C56 -0.5(4) . . . . ?
C54 C55 C56 C51 0.3(4) . . . . ?
C56 C51 C52 C53 -0.5(3) . . . . ?
N1 C1 C2 C3 -176.52(19) . . . . ?
N1 C6 C7 C8 -176.68(18) . . . . ?
N1 C6 C7 C12 3.6(3) . . . . ?
N1 C6 C11 C10 176.42(17) . . . . ?
N1 C6 C11 C15 -3.5(3) . . . . ?
N2 C18 C19 C20 174.49(18) . . . . ?
N2 C18 C19 C27 -4.7(3) . . . . ?
N2 C18 C23 C22 -174.27(18) . . . . ?
N2 C18 C23 C24 2.9(3) . . . . ?
S1 C38 C39 C40 51.2(2) . . . . ?
S1 C38 C39 C44 -132.06(18) . . . . ?
S1 C38 C45 C46 53.1(2) . . . . ?
S1 C38 C45 C50 -130.53(18) . . . . ?
S1 C38 C51 C52 43.7(2) . . . . ?
S1 C38 C51 C56 -143.84(17) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexamethyldisiloxane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bmkxr74
_database_code_depnum_ccdc_archive 'CCDC 2004177'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-15 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT112_bmkxr74             
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem       a/2         96 %Fit  
RESPONSE: We checked for a higher symmetry solution but the diffraction 
data could not be solved in a higher symmetry space group.  
;
# end Validation Reply Form
_audit_creation_date             2020-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            (BDI)Nb(NAr)(N(tBu)C(CPh2)O)
_chemical_name_systematic        
(N-tert-butylamino-2,2-diphenylethenolato-N,O)-(2,6-diisopropylphenyl)imino-(tert-butyl)imino-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-niobium(V)
_chemical_formula_moiety         'C51 H69 N4 Nb O'
_chemical_formula_sum            'C51 H69 N4 Nb O'
_chemical_formula_weight         847.01
_chemical_melting_point          423
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   24.1485(11)
_cell_length_b                   15.8759(7)
_cell_length_c                   24.2007(11)
_cell_angle_alpha                90
_cell_angle_beta                 101.813(2)
_cell_angle_gamma                90
_cell_volume                     9081.5(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.18
_shelx_estimated_absorpt_T_max   0.953
_shelx_estimated_absorpt_T_min   0.941
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0864 before and 0.0475 after correction.
The Ratio of minimum to maximum transmission is 0.9538.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            123296
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.441
_diffrn_reflns_theta_min         1.544
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12840
_reflns_number_total             16641
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.385
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1059
_refine_ls_number_reflns         16641
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0395
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0584P)²+6.4150P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1145
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C27(H27), C75(H75), C63(H63), C24(H24), C12(H12), C78(H78), C66(H66), C15(H15)
2.b Aromatic/amide H refined with riding coordinates:
 C53(H53), C2(H2), C61(H61), C92(H92), C51(H51), C93(H93), C60(H60), C10(H10),
 C72(H72), C9(H9), C41(H41), C20(H20), C73(H73), C102(H102), C59(H59), C8(H8),
 C21(H21), C22(H22), C71(H71), C42(H42), C100(H100), C96(H96), C95(H95),
 C94(H94), C49(H49), C50(H50), C43(H43), C101(H101), C98(H98), C99(H99),
 C45(H45), C48(H48), C47(H47), C44(H44)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C),
 C87(H87A,H87B,H87C), C25(H25A,H25B,H25C), C36(H36A,H36B,H36C), C88(H88A,H88B,
 H88C), C83(H83A,H83B,H83C), C37(H37A,H37B,H37C), C77(H77A,H77B,H77C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C33(H33A,H33B,H33C),
 C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C79(H79A,H79B,H79C), C82(H82A,H82B,
 H82C), C32(H32A,H32B,H32C), C13(H13A,H13B,H13C), C65(H65A,H65B,H65C), C67(H67A,
 H67B,H67C), C26(H26A,H26B,H26C), C76(H76A,H76B,H76C), C68(H68A,H68B,H68C),
 C64(H64A,H64B,H64C), C80(H80A,H80B,H80C), C31(H31A,H31B,H31C), C17(H17A,H17B,
 H17C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.36651(2) 0.18728(2) 0.64439(2) 0.01209(7) Uani 1 1 d . . . . .
Nb2 Nb 0.86850(2) 0.18881(2) 0.65073(2) 0.01179(7) Uani 1 1 d . . . . .
O1 O 0.31057(6) 0.18031(10) 0.56618(6) 0.0190(3) Uani 1 1 d . . . . .
O2 O 0.81171(6) 0.17834(10) 0.57336(6) 0.0193(3) Uani 1 1 d . . . . .
N2 N 0.28892(7) 0.24026(10) 0.66173(7) 0.0136(4) Uani 1 1 d . . . . .
N6 N 0.79093(7) 0.24024(11) 0.66920(7) 0.0138(4) Uani 1 1 d . . . . .
N5 N 0.90855(7) 0.30620(10) 0.67712(7) 0.0133(4) Uani 1 1 d . . . . .
N8 N 0.90177(7) 0.13730(11) 0.58776(7) 0.0152(4) Uani 1 1 d . . . . .
N4 N 0.39882(7) 0.13112(11) 0.58228(7) 0.0156(4) Uani 1 1 d . . . . .
N1 N 0.40639(7) 0.30443(11) 0.66992(7) 0.0137(4) Uani 1 1 d . . . . .
N7 N 0.88607(7) 0.12735(11) 0.71297(7) 0.0154(4) Uani 1 1 d . . . . .
N3 N 0.38319(7) 0.12704(11) 0.70753(7) 0.0162(4) Uani 1 1 d . . . . .
C54 C 0.79540(9) 0.28508(13) 0.71638(9) 0.0146(4) Uani 1 1 d . . . . .
C52 C 0.89273(9) 0.34913(13) 0.71920(9) 0.0150(4) Uani 1 1 d . . . . .
C58 C 1.00856(9) 0.29962(14) 0.66803(9) 0.0167(5) Uani 1 1 d . . . . .
C6 C 0.45497(9) 0.33333(13) 0.64846(9) 0.0146(4) Uani 1 1 d . . . . .
C3 C 0.29284(9) 0.28699(13) 0.70792(9) 0.0156(4) Uani 1 1 d . . . . .
C53 C 0.84509(9) 0.32999(13) 0.74132(9) 0.0164(5) Uani 1 1 d . . . . .
H53 H 0.846123 0.349976 0.778516 0.020 Uiso 1 1 calc R . . . .
C2 C 0.34313(9) 0.32970(14) 0.73404(9) 0.0171(5) Uani 1 1 d . . . . .
H2 H 0.343547 0.350383 0.770963 0.021 Uiso 1 1 calc R . . . .
C7 C 0.50942(9) 0.30387(14) 0.67333(9) 0.0173(5) Uani 1 1 d . . . . .
C1 C 0.39179(9) 0.34562(13) 0.71346(9) 0.0155(4) Uani 1 1 d . . . . .
C57 C 0.95467(9) 0.33737(13) 0.65244(9) 0.0148(4) Uani 1 1 d . . . . .
C61 C 0.98979(9) 0.42929(14) 0.58817(9) 0.0203(5) Uani 1 1 d . . . . .
H61 H 0.983894 0.473817 0.561384 0.024 Uiso 1 1 calc R . . . .
C38 C 0.35374(9) 0.16385(14) 0.54007(9) 0.0160(5) Uani 1 1 d . . . . .
C40 C 0.40392(9) 0.19555(14) 0.46202(9) 0.0182(5) Uani 1 1 d . . . . .
C27 C 0.23537(9) 0.07192(14) 0.66318(10) 0.0204(5) Uani 1 1 d . . . . .
H27 H 0.273306 0.091253 0.684103 0.025 Uiso 1 1 calc R . . . .
C91 C 0.90194(9) 0.20205(14) 0.46659(9) 0.0186(5) Uani 1 1 d . . . . .
C89 C 0.85457(9) 0.16681(14) 0.54620(9) 0.0157(5) Uani 1 1 d . . . . .
C69 C 0.73440(8) 0.22114(13) 0.63723(9) 0.0151(4) Uani 1 1 d . . . . .
C97 C 0.79555(9) 0.21416(14) 0.45591(9) 0.0187(5) Uani 1 1 d . . . . .
C90 C 0.85117(9) 0.18999(13) 0.49144(9) 0.0172(5) Uani 1 1 d . . . . .
C74 C 0.70921(9) 0.14270(14) 0.64270(9) 0.0182(5) Uani 1 1 d . . . . .
C92 C 0.94640(9) 0.25381(14) 0.49316(9) 0.0211(5) Uani 1 1 d . . . . .
H92 H 0.944804 0.278584 0.528532 0.025 Uiso 1 1 calc R . . . .
C46 C 0.29692(9) 0.20951(15) 0.44840(9) 0.0195(5) Uani 1 1 d . . . . .
C51 C 0.24581(10) 0.17075(15) 0.45302(10) 0.0223(5) Uani 1 1 d . . . . .
H51 H 0.246112 0.127009 0.479866 0.027 Uiso 1 1 calc R . . . .
C39 C 0.35192(9) 0.18550(13) 0.48514(9) 0.0178(5) Uani 1 1 d . . . . .
C75 C 0.73599(9) 0.36301(14) 0.58744(9) 0.0208(5) Uani 1 1 d . . . . .
H75 H 0.777724 0.352847 0.597034 0.025 Uiso 1 1 calc R . . . .
C93 C 0.99252(10) 0.26972(15) 0.46916(10) 0.0247(5) Uani 1 1 d . . . . .
H93 H 1.022054 0.305349 0.487938 0.030 Uiso 1 1 calc R . . . .
C63 C 1.02198(9) 0.23329(15) 0.71429(10) 0.0210(5) Uani 1 1 d . . . . .
H63 H 0.986926 0.199369 0.713487 0.025 Uiso 1 1 calc R . . . .
C62 C 0.94495(9) 0.40301(14) 0.61291(9) 0.0184(5) Uani 1 1 d . . . . .
C60 C 1.04202(9) 0.39177(15) 0.60202(9) 0.0209(5) Uani 1 1 d . . . . .
H60 H 1.071787 0.409914 0.584559 0.025 Uiso 1 1 calc R . . . .
C10 C 0.49444(9) 0.41877(14) 0.58403(9) 0.0211(5) Uani 1 1 d . . . . .
H10 H 0.490001 0.458784 0.554258 0.025 Uiso 1 1 calc R . . . .
C72 C 0.62628(10) 0.18816(14) 0.57581(10) 0.0229(5) Uani 1 1 d . . . . .
H72 H 0.588684 0.177969 0.555966 0.027 Uiso 1 1 calc R . . . .
C70 C 0.70706(9) 0.28139(14) 0.59900(9) 0.0171(5) Uani 1 1 d . . . . .
C4 C 0.42914(9) 0.41670(14) 0.74113(9) 0.0203(5) Uani 1 1 d . . . . .
H4A H 0.467338 0.395207 0.755919 0.030 Uiso 1 1 calc GR . . . .
H4B H 0.413503 0.440058 0.772169 0.030 Uiso 1 1 calc GR . . . .
H4C H 0.430761 0.460880 0.713227 0.030 Uiso 1 1 calc GR . . . .
C9 C 0.54778(9) 0.38985(15) 0.60767(9) 0.0213(5) Uani 1 1 d . . . . .
H9 H 0.579606 0.409449 0.593936 0.026 Uiso 1 1 calc R . . . .
C24 C 0.23526(9) 0.37250(14) 0.58548(9) 0.0192(5) Uani 1 1 d . . . . .
H24 H 0.273891 0.371051 0.610186 0.023 Uiso 1 1 calc R . . . .
C19 C 0.20636(9) 0.28899(14) 0.59217(9) 0.0161(5) Uani 1 1 d . . . . .
C23 C 0.20700(9) 0.14546(14) 0.62815(9) 0.0174(5) Uani 1 1 d . . . . .
C5 C 0.24160(9) 0.30095(14) 0.73405(10) 0.0201(5) Uani 1 1 d . . . . .
H5A H 0.217324 0.344278 0.712666 0.030 Uiso 1 1 calc GR . . . .
H5B H 0.254025 0.319379 0.773277 0.030 Uiso 1 1 calc GR . . . .
H5C H 0.220339 0.248202 0.733077 0.030 Uiso 1 1 calc GR . . . .
C41 C 0.45046(9) 0.23976(15) 0.49243(9) 0.0219(5) Uani 1 1 d . . . . .
H41 H 0.449494 0.259379 0.529310 0.026 Uiso 1 1 calc R . . . .
C20 C 0.15329(9) 0.27324(15) 0.55864(9) 0.0201(5) Uani 1 1 d . . . . .
H20 H 0.134880 0.316441 0.534522 0.024 Uiso 1 1 calc R . . . .
C18 C 0.23268(9) 0.22465(14) 0.62779(9) 0.0154(4) Uani 1 1 d . . . . .
C55 C 0.92544(9) 0.42665(14) 0.74256(9) 0.0204(5) Uani 1 1 d . . . . .
H55A H 0.965782 0.417787 0.743499 0.031 Uiso 1 1 calc GR . . . .
H55B H 0.919794 0.437415 0.780897 0.031 Uiso 1 1 calc GR . . . .
H55C H 0.911989 0.475124 0.718452 0.031 Uiso 1 1 calc GR . . . .
C73 C 0.65460(9) 0.12815(15) 0.61148(10) 0.0233(5) Uani 1 1 d . . . . .
H73 H 0.636774 0.075660 0.615069 0.028 Uiso 1 1 calc R . . . .
C102 C 0.74471(9) 0.17524(15) 0.46114(10) 0.0223(5) Uani 1 1 d . . . . .
H102 H 0.745337 0.131436 0.488001 0.027 Uiso 1 1 calc R . . . .
C59 C 1.05125(9) 0.32747(14) 0.64145(9) 0.0195(5) Uani 1 1 d . . . . .
H59 H 1.087483 0.301725 0.650607 0.023 Uiso 1 1 calc R . . . .
C8 C 0.55500(9) 0.33226(15) 0.65141(10) 0.0212(5) Uani 1 1 d . . . . .
H8 H 0.591859 0.311647 0.666821 0.025 Uiso 1 1 calc R . . . .
C21 C 0.12666(9) 0.19620(14) 0.55958(10) 0.0222(5) Uani 1 1 d . . . . .
H21 H 0.090208 0.186853 0.536778 0.027 Uiso 1 1 calc R . . . .
C30 C 0.38828(9) 0.07975(14) 0.76031(9) 0.0190(5) Uani 1 1 d . . . . .
C22 C 0.15376(9) 0.13325(14) 0.59403(9) 0.0212(5) Uani 1 1 d . . . . .
H22 H 0.135652 0.080205 0.594513 0.025 Uiso 1 1 calc R . . . .
C71 C 0.65276(9) 0.26394(15) 0.56879(9) 0.0216(5) Uani 1 1 d . . . . .
H71 H 0.633508 0.304498 0.542961 0.026 Uiso 1 1 calc R . . . .
C12 C 0.52078(9) 0.24346(15) 0.72326(10) 0.0231(5) Uani 1 1 d . . . . .
H12 H 0.483745 0.229099 0.733296 0.028 Uiso 1 1 calc R . . . .
C78 C 0.73895(10) 0.07160(14) 0.67879(10) 0.0221(5) Uani 1 1 d . . . . .
H78 H 0.777156 0.092178 0.698108 0.026 Uiso 1 1 calc R . . . .
C42 C 0.49787(10) 0.25565(15) 0.47016(10) 0.0249(5) Uani 1 1 d . . . . .
H42 H 0.528817 0.285979 0.491706 0.030 Uiso 1 1 calc R . . . .
C56 C 0.74568(9) 0.29403(14) 0.74532(9) 0.0199(5) Uani 1 1 d . . . . .
H56A H 0.716049 0.327802 0.721618 0.030 Uiso 1 1 calc GR . . . .
H56B H 0.758148 0.321964 0.781865 0.030 Uiso 1 1 calc GR . . . .
H56C H 0.730684 0.238117 0.751198 0.030 Uiso 1 1 calc GR . . . .
C81 C 0.89471(9) 0.07996(14) 0.76602(9) 0.0192(5) Uani 1 1 d . . . . .
C100 C 0.69145(10) 0.26418(17) 0.38835(10) 0.0307(6) Uani 1 1 d . . . . .
H100 H 0.656310 0.280996 0.365638 0.037 Uiso 1 1 calc R . . . .
C85 C 0.93432(9) 0.06052(14) 0.57733(9) 0.0192(5) Uani 1 1 d . . . . .
C96 C 0.90575(10) 0.16765(15) 0.41434(10) 0.0226(5) Uani 1 1 d . . . . .
H96 H 0.875991 0.133032 0.394831 0.027 Uiso 1 1 calc R . . . .
C95 C 0.95225(10) 0.18325(16) 0.39057(10) 0.0263(6) Uani 1 1 d . . . . .
H95 H 0.954149 0.158847 0.355169 0.032 Uiso 1 1 calc R . . . .
C94 C 0.99583(10) 0.23383(16) 0.41774(10) 0.0273(6) Uani 1 1 d . . . . .
H94 H 1.027769 0.243960 0.401390 0.033 Uiso 1 1 calc R . . . .
C87 C 0.98964(10) 0.08345(16) 0.55878(10) 0.0271(6) Uani 1 1 d . . . . .
H87A H 0.981208 0.100216 0.518968 0.041 Uiso 1 1 calc GR . . . .
H87B H 1.014899 0.034506 0.563690 0.041 Uiso 1 1 calc GR . . . .
H87C H 1.008063 0.130251 0.581870 0.041 Uiso 1 1 calc GR . . . .
C25 C 0.24208(11) 0.38241(15) 0.52453(10) 0.0274(6) Uani 1 1 d . . . . .
H25A H 0.263887 0.334873 0.514365 0.041 Uiso 1 1 calc GR . . . .
H25B H 0.262055 0.435125 0.520658 0.041 Uiso 1 1 calc GR . . . .
H25C H 0.204687 0.383592 0.499423 0.041 Uiso 1 1 calc GR . . . .
C49 C 0.19323(10) 0.25827(16) 0.37944(10) 0.0276(6) Uani 1 1 d . . . . .
H49 H 0.158228 0.274370 0.356140 0.033 Uiso 1 1 calc R . . . .
C11 C 0.44671(9) 0.39061(14) 0.60284(9) 0.0195(5) Uani 1 1 d . . . . .
C50 C 0.19508(10) 0.19506(15) 0.41924(10) 0.0265(6) Uani 1 1 d . . . . .
H50 H 0.161039 0.168097 0.423343 0.032 Uiso 1 1 calc R . . . .
C43 C 0.50028(10) 0.22741(17) 0.41654(10) 0.0285(6) Uani 1 1 d . . . . .
H43 H 0.532802 0.237851 0.401160 0.034 Uiso 1 1 calc R . . . .
C101 C 0.69349(10) 0.19978(16) 0.42766(11) 0.0277(6) Uani 1 1 d . . . . .
H101 H 0.659563 0.172348 0.431637 0.033 Uiso 1 1 calc R . . . .
C98 C 0.79269(10) 0.27846(15) 0.41581(9) 0.0220(5) Uani 1 1 d . . . . .
H98 H 0.826505 0.305523 0.411110 0.026 Uiso 1 1 calc R . . . .
C36 C 0.48753(10) 0.06790(16) 0.56094(10) 0.0262(5) Uani 1 1 d . . . . .
H36A H 0.484173 0.090984 0.522843 0.039 Uiso 1 1 calc GR . . . .
H36B H 0.509143 0.015255 0.564138 0.039 Uiso 1 1 calc GR . . . .
H36C H 0.507093 0.108557 0.588670 0.039 Uiso 1 1 calc GR . . . .
C99 C 0.74105(10) 0.30348(16) 0.38263(10) 0.0259(6) Uani 1 1 d . . . . .
H99 H 0.739975 0.347726 0.356004 0.031 Uiso 1 1 calc R . . . .
C45 C 0.40719(10) 0.16822(16) 0.40802(10) 0.0248(5) Uani 1 1 d . . . . .
H45 H 0.376254 0.138324 0.386102 0.030 Uiso 1 1 calc R . . . .
C88 C 0.89861(10) 0.00301(15) 0.53368(10) 0.0280(6) Uani 1 1 d . . . . .
H88A H 0.862854 -0.009626 0.545117 0.042 Uiso 1 1 calc GR . . . .
H88B H 0.919210 -0.049515 0.530971 0.042 Uiso 1 1 calc GR . . . .
H88C H 0.890797 0.031171 0.496864 0.042 Uiso 1 1 calc GR . . . .
C48 C 0.24292(10) 0.29769(16) 0.37401(10) 0.0254(5) Uani 1 1 d . . . . .
H48 H 0.242046 0.341445 0.347066 0.030 Uiso 1 1 calc R . . . .
C34 C 0.42835(9) 0.05053(14) 0.57216(9) 0.0206(5) Uani 1 1 d . . . . .
C83 C 0.87672(10) -0.01188(14) 0.75569(10) 0.0257(5) Uani 1 1 d . . . . .
H83A H 0.836626 -0.014310 0.737315 0.039 Uiso 1 1 calc GR . . . .
H83B H 0.882522 -0.041837 0.791827 0.039 Uiso 1 1 calc GR . . . .
H83C H 0.899467 -0.038429 0.731304 0.039 Uiso 1 1 calc GR . . . .
C66 C 0.88796(10) 0.44669(15) 0.59419(10) 0.0251(5) Uani 1 1 d . . . . .
H66 H 0.861530 0.424356 0.617544 0.030 Uiso 1 1 calc R . . . .
C47 C 0.29433(10) 0.27341(15) 0.40796(9) 0.0227(5) Uani 1 1 d . . . . .
H47 H 0.328192 0.300689 0.403604 0.027 Uiso 1 1 calc R . . . .
C37 C 0.39390(11) -0.00002(15) 0.52334(10) 0.0281(6) Uani 1 1 d . . . . .
H37A H 0.355449 -0.008261 0.529646 0.042 Uiso 1 1 calc GR . . . .
H37B H 0.411833 -0.054949 0.521116 0.042 Uiso 1 1 calc GR . . . .
H37C H 0.392282 0.030677 0.487915 0.042 Uiso 1 1 calc GR . . . .
C77 C 0.72068(12) 0.38647(16) 0.52510(10) 0.0324(6) Uani 1 1 d . . . . .
H77A H 0.730346 0.339743 0.502363 0.049 Uiso 1 1 calc GR . . . .
H77B H 0.741832 0.436854 0.518440 0.049 Uiso 1 1 calc GR . . . .
H77C H 0.680007 0.397918 0.514420 0.049 Uiso 1 1 calc GR . . . .
C44 C 0.45464(11) 0.18379(17) 0.38570(11) 0.0307(6) Uani 1 1 d . . . . .
H44 H 0.455858 0.164322 0.348848 0.037 Uiso 1 1 calc R . . . .
C28 C 0.24459(11) -0.00121(15) 0.62478(11) 0.0300(6) Uani 1 1 d . . . . .
H28A H 0.207923 -0.021005 0.603547 0.045 Uiso 1 1 calc GR . . . .
H28B H 0.263954 -0.047381 0.647832 0.045 Uiso 1 1 calc GR . . . .
H28C H 0.267777 0.017958 0.598397 0.045 Uiso 1 1 calc GR . . . .
C29 C 0.20140(10) 0.04309(16) 0.70666(11) 0.0298(6) Uani 1 1 d . . . . .
H29A H 0.196723 0.090432 0.731283 0.045 Uiso 1 1 calc GR . . . .
H29B H 0.221601 -0.002721 0.729429 0.045 Uiso 1 1 calc GR . . . .
H29C H 0.164131 0.023088 0.687105 0.045 Uiso 1 1 calc GR . . . .
C35 C 0.43370(11) -0.00316(15) 0.62560(10) 0.0299(6) Uani 1 1 d . . . . .
H35A H 0.455705 0.027598 0.657853 0.045 Uiso 1 1 calc GR . . . .
H35B H 0.452898 -0.056152 0.620580 0.045 Uiso 1 1 calc GR . . . .
H35C H 0.395918 -0.015281 0.632536 0.045 Uiso 1 1 calc GR . . . .
C15 C 0.38846(10) 0.42084(16) 0.57295(10) 0.0287(6) Uani 1 1 d . . . . .
H15 H 0.361113 0.374574 0.575900 0.034 Uiso 1 1 calc R . . . .
C33 C 0.36751(10) -0.01078(14) 0.74923(10) 0.0262(5) Uani 1 1 d . . . . .
H33A H 0.327796 -0.010414 0.729485 0.039 Uiso 1 1 calc GR . . . .
H33B H 0.370977 -0.040606 0.785230 0.039 Uiso 1 1 calc GR . . . .
H33C H 0.390429 -0.039387 0.725869 0.039 Uiso 1 1 calc GR . . . .
C84 C 0.95770(10) 0.08419(17) 0.79408(10) 0.0297(6) Uani 1 1 d . . . . .
H84A H 0.980308 0.060681 0.768456 0.045 Uiso 1 1 calc GR . . . .
H84B H 0.964401 0.051597 0.829207 0.045 Uiso 1 1 calc GR . . . .
H84C H 0.968606 0.142998 0.802483 0.045 Uiso 1 1 calc GR . . . .
C86 C 0.94979(11) 0.01279(16) 0.63337(10) 0.0306(6) Uani 1 1 d . . . . .
H86A H 0.971989 0.049560 0.662148 0.046 Uiso 1 1 calc GR . . . .
H86B H 0.972140 -0.037152 0.628458 0.046 Uiso 1 1 calc GR . . . .
H86C H 0.915125 -0.004582 0.645364 0.046 Uiso 1 1 calc GR . . . .
C79 C 0.70671(11) 0.04467(16) 0.72446(11) 0.0316(6) Uani 1 1 d . . . . .
H79A H 0.701229 0.093656 0.747386 0.047 Uiso 1 1 calc GR . . . .
H79B H 0.728553 0.001663 0.748641 0.047 Uiso 1 1 calc GR . . . .
H79C H 0.669801 0.021505 0.706465 0.047 Uiso 1 1 calc GR . . . .
C82 C 0.86033(10) 0.12095(15) 0.80591(9) 0.0242(5) Uani 1 1 d . . . . .
H82A H 0.872196 0.179692 0.812862 0.036 Uiso 1 1 calc GR . . . .
H82B H 0.866945 0.090184 0.841769 0.036 Uiso 1 1 calc GR . . . .
H82C H 0.819969 0.119048 0.788479 0.036 Uiso 1 1 calc GR . . . .
C32 C 0.35291(11) 0.12363(15) 0.79776(10) 0.0277(6) Uani 1 1 d . . . . .
H32A H 0.367853 0.180365 0.807265 0.042 Uiso 1 1 calc GR . . . .
H32B H 0.354797 0.091059 0.832490 0.042 Uiso 1 1 calc GR . . . .
H32C H 0.313481 0.127510 0.777438 0.042 Uiso 1 1 calc GR . . . .
C13 C 0.55913(11) 0.28253(17) 0.77540(10) 0.0333(6) Uani 1 1 d . . . . .
H13A H 0.597248 0.290276 0.768097 0.050 Uiso 1 1 calc GR . . . .
H13B H 0.560860 0.245032 0.807873 0.050 Uiso 1 1 calc GR . . . .
H13C H 0.543752 0.337231 0.783512 0.050 Uiso 1 1 calc GR . . . .
C65 C 1.06926(11) 0.17254(16) 0.70726(11) 0.0313(6) Uani 1 1 d . . . . .
H65A H 1.061032 0.149018 0.669016 0.047 Uiso 1 1 calc GR . . . .
H65B H 1.071694 0.126796 0.734849 0.047 Uiso 1 1 calc GR . . . .
H65C H 1.105339 0.202902 0.713431 0.047 Uiso 1 1 calc GR . . . .
C67 C 0.89230(11) 0.54275(16) 0.60244(11) 0.0339(6) Uani 1 1 d . . . . .
H67A H 0.912243 0.555364 0.641039 0.051 Uiso 1 1 calc GR . . . .
H67B H 0.854228 0.567098 0.595979 0.051 Uiso 1 1 calc GR . . . .
H67C H 0.913207 0.566963 0.575554 0.051 Uiso 1 1 calc GR . . . .
C26 C 0.20346(11) 0.44813(15) 0.60343(11) 0.0302(6) Uani 1 1 d . . . . .
H26A H 0.165931 0.452240 0.578759 0.045 Uiso 1 1 calc GR . . . .
H26B H 0.224784 0.499860 0.600411 0.045 Uiso 1 1 calc GR . . . .
H26C H 0.199354 0.440580 0.642584 0.045 Uiso 1 1 calc GR . . . .
C76 C 0.72352(12) 0.43660(16) 0.62359(11) 0.0357(6) Uani 1 1 d . . . . .
H76A H 0.682799 0.448235 0.615228 0.054 Uiso 1 1 calc GR . . . .
H76B H 0.744055 0.486639 0.615145 0.054 Uiso 1 1 calc GR . . . .
H76C H 0.735686 0.422176 0.663612 0.054 Uiso 1 1 calc GR . . . .
C68 C 0.86351(11) 0.42564(17) 0.53235(10) 0.0330(6) Uani 1 1 d . . . . .
H68A H 0.891185 0.439993 0.509356 0.049 Uiso 1 1 calc GR . . . .
H68B H 0.828775 0.458106 0.519322 0.049 Uiso 1 1 calc GR . . . .
H68C H 0.854902 0.365319 0.528727 0.049 Uiso 1 1 calc GR . . . .
C64 C 1.03857(12) 0.27367(17) 0.77239(10) 0.0332(6) Uani 1 1 d . . . . .
H64A H 1.071252 0.310641 0.773387 0.050 Uiso 1 1 calc GR . . . .
H64B H 1.048387 0.229589 0.801072 0.050 Uiso 1 1 calc GR . . . .
H64C H 1.006738 0.306758 0.780104 0.050 Uiso 1 1 calc GR . . . .
C80 C 0.74730(11) -0.00330(15) 0.64136(11) 0.0321(6) Uani 1 1 d . . . . .
H80A H 0.710322 -0.025436 0.622663 0.048 Uiso 1 1 calc GR . . . .
H80B H 0.768752 -0.047525 0.664698 0.048 Uiso 1 1 calc GR . . . .
H80C H 0.768177 0.015180 0.612808 0.048 Uiso 1 1 calc GR . . . .
C31 C 0.45042(10) 0.07908(18) 0.79070(11) 0.0338(6) Uani 1 1 d . . . . .
H31A H 0.473320 0.052510 0.766469 0.051 Uiso 1 1 calc GR . . . .
H31B H 0.454368 0.047238 0.825987 0.051 Uiso 1 1 calc GR . . . .
H31C H 0.463378 0.137050 0.799120 0.051 Uiso 1 1 calc GR . . . .
C17 C 0.38500(11) 0.43725(17) 0.51020(10) 0.0329(6) Uani 1 1 d . . . . .
H17A H 0.345379 0.445181 0.491392 0.049 Uiso 1 1 calc GR . . . .
H17B H 0.400789 0.389029 0.493383 0.049 Uiso 1 1 calc GR . . . .
H17C H 0.406631 0.488058 0.505532 0.049 Uiso 1 1 calc GR . . . .
C14 C 0.54806(13) 0.16187(17) 0.70884(12) 0.0385(7) Uani 1 1 d . . . . .
H14A H 0.521916 0.132364 0.678738 0.058 Uiso 1 1 calc GR . . . .
H14B H 0.556682 0.125915 0.742425 0.058 Uiso 1 1 calc GR . . . .
H14C H 0.583089 0.174916 0.696106 0.058 Uiso 1 1 calc GR . . . .
C16 C 0.36971(12) 0.49711(19) 0.60123(11) 0.0439(7) Uani 1 1 d . . . . .
H16A H 0.365411 0.482135 0.639409 0.066 Uiso 1 1 calc GR . . . .
H16B H 0.333411 0.517106 0.579303 0.066 Uiso 1 1 calc GR . . . .
H16C H 0.398115 0.541732 0.603382 0.066 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O1 2.0910(15) . ?
Nb1 N2 2.1718(17) . ?
Nb1 N4 2.0353(17) . ?
Nb1 N1 2.1271(17) . ?
Nb1 N3 1.7777(17) . ?
Nb1 C38 2.507(2) . ?
Nb2 O2 2.0888(15) . ?
Nb2 N6 2.1721(17) . ?
Nb2 N5 2.1363(17) . ?
Nb2 N8 2.0342(17) . ?
Nb2 N7 1.7718(17) . ?
Nb2 C89 2.507(2) . ?
O1 C38 1.351(3) . ?
O2 C89 1.347(3) . ?
N2 C3 1.329(3) . ?
N2 C18 1.457(3) . ?
N6 C54 1.331(3) . ?
N6 C69 1.457(3) . ?
N5 C52 1.344(3) . ?
N5 C57 1.454(3) . ?
N8 C89 1.436(3) . ?
N8 C85 1.500(3) . ?
N4 C38 1.429(3) . ?
N4 C34 1.509(3) . ?
N1 C6 1.451(3) . ?
N1 C1 1.347(3) . ?
N7 C81 1.466(3) . ?
N3 C30 1.465(3) . ?
C54 C53 1.420(3) . ?
C54 C56 1.515(3) . ?
C52 C53 1.398(3) . ?
C52 C55 1.508(3) . ?
C58 C57 1.412(3) . ?
C58 C63 1.523(3) . ?
C58 C59 1.394(3) . ?
C6 C7 1.409(3) . ?
C6 C11 1.412(3) . ?
C3 C2 1.421(3) . ?
C3 C5 1.517(3) . ?
C53 H53 0.9500 . ?
C2 H2 0.9500 . ?
C2 C1 1.390(3) . ?
C7 C8 1.391(3) . ?
C7 C12 1.523(3) . ?
C1 C4 1.512(3) . ?
C57 C62 1.402(3) . ?
C61 H61 0.9500 . ?
C61 C62 1.404(3) . ?
C61 C60 1.373(3) . ?
C38 C39 1.365(3) . ?
C40 C39 1.484(3) . ?
C40 C41 1.399(3) . ?
C40 C45 1.394(3) . ?
C27 H27 1.0000 . ?
C27 C23 1.521(3) . ?
C27 C28 1.532(3) . ?
C27 C29 1.531(3) . ?
C91 C90 1.484(3) . ?
C91 C92 1.400(3) . ?
C91 C96 1.398(3) . ?
C89 C90 1.361(3) . ?
C69 C74 1.404(3) . ?
C69 C70 1.399(3) . ?
C97 C90 1.489(3) . ?
C97 C102 1.403(3) . ?
C97 C98 1.400(3) . ?
C74 C73 1.398(3) . ?
C74 C78 1.515(3) . ?
C92 H92 0.9500 . ?
C92 C93 1.381(3) . ?
C46 C51 1.404(3) . ?
C46 C39 1.489(3) . ?
C46 C47 1.402(3) . ?
C51 H51 0.9500 . ?
C51 C50 1.381(3) . ?
C75 H75 1.0000 . ?
C75 C70 1.525(3) . ?
C75 C77 1.524(3) . ?
C75 C76 1.526(3) . ?
C93 H93 0.9500 . ?
C93 C94 1.386(3) . ?
C63 H63 1.0000 . ?
C63 C65 1.531(3) . ?
C63 C64 1.522(3) . ?
C62 C66 1.525(3) . ?
C60 H60 0.9500 . ?
C60 C59 1.384(3) . ?
C10 H10 0.9500 . ?
C10 C9 1.377(3) . ?
C10 C11 1.397(3) . ?
C72 H72 0.9500 . ?
C72 C73 1.371(3) . ?
C72 C71 1.389(3) . ?
C70 C71 1.392(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C9 H9 0.9500 . ?
C9 C8 1.382(3) . ?
C24 H24 1.0000 . ?
C24 C19 1.522(3) . ?
C24 C25 1.525(3) . ?
C24 C26 1.535(3) . ?
C19 C20 1.392(3) . ?
C19 C18 1.402(3) . ?
C23 C18 1.403(3) . ?
C23 C22 1.392(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C41 H41 0.9500 . ?
C41 C42 1.385(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.384(3) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C73 H73 0.9500 . ?
C102 H102 0.9500 . ?
C102 C101 1.388(3) . ?
C59 H59 0.9500 . ?
C8 H8 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.378(3) . ?
C30 C33 1.528(3) . ?
C30 C32 1.534(3) . ?
C30 C31 1.530(3) . ?
C22 H22 0.9500 . ?
C71 H71 0.9500 . ?
C12 H12 1.0000 . ?
C12 C13 1.535(3) . ?
C12 C14 1.526(4) . ?
C78 H78 1.0000 . ?
C78 C79 1.537(3) . ?
C78 C80 1.533(3) . ?
C42 H42 0.9500 . ?
C42 C43 1.385(3) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C81 C83 1.527(3) . ?
C81 C84 1.535(3) . ?
C81 C82 1.541(3) . ?
C100 H100 0.9500 . ?
C100 C101 1.390(4) . ?
C100 C99 1.382(4) . ?
C85 C87 1.537(3) . ?
C85 C88 1.523(3) . ?
C85 C86 1.532(3) . ?
C96 H96 0.9500 . ?
C96 C95 1.385(3) . ?
C95 H95 0.9500 . ?
C95 C94 1.379(3) . ?
C94 H94 0.9500 . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C49 H49 0.9500 . ?
C49 C50 1.385(4) . ?
C49 C48 1.383(4) . ?
C11 C15 1.522(3) . ?
C50 H50 0.9500 . ?
C43 H43 0.9500 . ?
C43 C44 1.384(4) . ?
C101 H101 0.9500 . ?
C98 H98 0.9500 . ?
C98 C99 1.396(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C36 C34 1.533(3) . ?
C99 H99 0.9500 . ?
C45 H45 0.9500 . ?
C45 C44 1.386(3) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C48 H48 0.9500 . ?
C48 C47 1.396(3) . ?
C34 C37 1.526(3) . ?
C34 C35 1.532(3) . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C66 H66 1.0000 . ?
C66 C67 1.539(3) . ?
C66 C68 1.529(3) . ?
C47 H47 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C44 H44 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C17 1.526(3) . ?
C15 C16 1.505(4) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nb1 N2 76.84(6) . . ?
O1 Nb1 N1 118.65(6) . . ?
O1 Nb1 C38 32.58(6) . . ?
N2 Nb1 C38 108.59(6) . . ?
N4 Nb1 O1 65.34(6) . . ?
N4 Nb1 N2 142.06(7) . . ?
N4 Nb1 N1 112.24(7) . . ?
N4 Nb1 C38 34.75(7) . . ?
N1 Nb1 N2 87.85(6) . . ?
N1 Nb1 C38 112.16(7) . . ?
N3 Nb1 O1 137.75(7) . . ?
N3 Nb1 N2 95.44(7) . . ?
N3 Nb1 N4 110.21(7) . . ?
N3 Nb1 N1 102.20(7) . . ?
N3 Nb1 C38 138.17(8) . . ?
O2 Nb2 N6 77.22(6) . . ?
O2 Nb2 N5 120.76(6) . . ?
O2 Nb2 C89 32.50(6) . . ?
N6 Nb2 C89 108.47(7) . . ?
N5 Nb2 N6 88.12(6) . . ?
N5 Nb2 C89 112.47(7) . . ?
N8 Nb2 O2 65.42(6) . . ?
N8 Nb2 N6 142.63(7) . . ?
N8 Nb2 N5 110.53(7) . . ?
N8 Nb2 C89 34.92(7) . . ?
N7 Nb2 O2 135.83(7) . . ?
N7 Nb2 N6 95.66(7) . . ?
N7 Nb2 N5 102.20(7) . . ?
N7 Nb2 N8 110.67(7) . . ?
N7 Nb2 C89 137.76(8) . . ?
C38 O1 Nb1 90.93(12) . . ?
C89 O2 Nb2 91.10(11) . . ?
C3 N2 Nb1 117.58(13) . . ?
C3 N2 C18 117.83(17) . . ?
C18 N2 Nb1 124.51(13) . . ?
C54 N6 Nb2 117.11(13) . . ?
C54 N6 C69 118.01(17) . . ?
C69 N6 Nb2 124.49(13) . . ?
C52 N5 Nb2 119.16(14) . . ?
C52 N5 C57 119.94(17) . . ?
C57 N5 Nb2 120.80(13) . . ?
C89 N8 Nb2 90.86(12) . . ?
C89 N8 C85 121.04(17) . . ?
C85 N8 Nb2 138.93(14) . . ?
C38 N4 Nb1 91.00(12) . . ?
C38 N4 C34 120.55(17) . . ?
C34 N4 Nb1 139.17(14) . . ?
C6 N1 Nb1 121.57(13) . . ?
C1 N1 Nb1 118.44(14) . . ?
C1 N1 C6 119.13(17) . . ?
C81 N7 Nb2 173.59(15) . . ?
C30 N3 Nb1 171.52(15) . . ?
N6 C54 C53 123.10(19) . . ?
N6 C54 C56 120.92(19) . . ?
C53 C54 C56 115.92(19) . . ?
N5 C52 C53 124.31(19) . . ?
N5 C52 C55 119.29(19) . . ?
C53 C52 C55 116.28(19) . . ?
C57 C58 C63 122.4(2) . . ?
C59 C58 C57 118.1(2) . . ?
C59 C58 C63 119.50(19) . . ?
C7 C6 N1 119.61(19) . . ?
C7 C6 C11 121.2(2) . . ?
C11 C6 N1 119.21(18) . . ?
N2 C3 C2 123.23(19) . . ?
N2 C3 C5 120.56(19) . . ?
C2 C3 C5 116.14(19) . . ?
C54 C53 H53 115.2 . . ?
C52 C53 C54 129.5(2) . . ?
C52 C53 H53 115.2 . . ?
C3 C2 H2 115.3 . . ?
C1 C2 C3 129.4(2) . . ?
C1 C2 H2 115.3 . . ?
C6 C7 C12 123.3(2) . . ?
C8 C7 C6 118.1(2) . . ?
C8 C7 C12 118.58(19) . . ?
N1 C1 C2 124.6(2) . . ?
N1 C1 C4 118.73(19) . . ?
C2 C1 C4 116.63(19) . . ?
C58 C57 N5 119.16(19) . . ?
C62 C57 N5 119.88(18) . . ?
C62 C57 C58 120.9(2) . . ?
C62 C61 H61 119.4 . . ?
C60 C61 H61 119.4 . . ?
C60 C61 C62 121.2(2) . . ?
O1 C38 Nb1 56.49(10) . . ?
O1 C38 N4 106.49(17) . . ?
O1 C38 C39 122.20(19) . . ?
N4 C38 Nb1 54.25(10) . . ?
C39 C38 Nb1 156.33(17) . . ?
C39 C38 N4 131.0(2) . . ?
C41 C40 C39 120.4(2) . . ?
C45 C40 C39 122.3(2) . . ?
C45 C40 C41 117.1(2) . . ?
C23 C27 H27 107.9 . . ?
C23 C27 C28 110.40(19) . . ?
C23 C27 C29 111.67(18) . . ?
C28 C27 H27 107.9 . . ?
C29 C27 H27 107.9 . . ?
C29 C27 C28 110.81(19) . . ?
C92 C91 C90 120.6(2) . . ?
C96 C91 C90 121.9(2) . . ?
C96 C91 C92 117.3(2) . . ?
O2 C89 Nb2 56.40(10) . . ?
O2 C89 N8 106.35(17) . . ?
O2 C89 C90 122.60(19) . . ?
N8 C89 Nb2 54.21(10) . . ?
C90 C89 Nb2 155.96(16) . . ?
C90 C89 N8 130.6(2) . . ?
C74 C69 N6 120.77(19) . . ?
C70 C69 N6 118.24(18) . . ?
C70 C69 C74 120.92(19) . . ?
C102 C97 C90 122.5(2) . . ?
C98 C97 C90 119.9(2) . . ?
C98 C97 C102 117.6(2) . . ?
C91 C90 C97 117.06(19) . . ?
C89 C90 C91 122.6(2) . . ?
C89 C90 C97 119.9(2) . . ?
C69 C74 C78 123.49(19) . . ?
C73 C74 C69 118.3(2) . . ?
C73 C74 C78 118.1(2) . . ?
C91 C92 H92 119.2 . . ?
C93 C92 C91 121.5(2) . . ?
C93 C92 H92 119.2 . . ?
C51 C46 C39 122.1(2) . . ?
C47 C46 C51 117.3(2) . . ?
C47 C46 C39 120.6(2) . . ?
C46 C51 H51 119.4 . . ?
C50 C51 C46 121.2(2) . . ?
C50 C51 H51 119.4 . . ?
C38 C39 C40 122.2(2) . . ?
C38 C39 C46 119.5(2) . . ?
C40 C39 C46 117.87(19) . . ?
C70 C75 H75 107.3 . . ?
C70 C75 C76 113.2(2) . . ?
C77 C75 H75 107.3 . . ?
C77 C75 C70 111.22(19) . . ?
C77 C75 C76 110.1(2) . . ?
C76 C75 H75 107.3 . . ?
C92 C93 H93 119.9 . . ?
C92 C93 C94 120.2(2) . . ?
C94 C93 H93 119.9 . . ?
C58 C63 H63 107.8 . . ?
C58 C63 C65 113.92(19) . . ?
C65 C63 H63 107.8 . . ?
C64 C63 C58 111.34(19) . . ?
C64 C63 H63 107.8 . . ?
C64 C63 C65 107.86(19) . . ?
C57 C62 C61 118.4(2) . . ?
C57 C62 C66 123.8(2) . . ?
C61 C62 C66 117.8(2) . . ?
C61 C60 H60 120.1 . . ?
C61 C60 C59 119.9(2) . . ?
C59 C60 H60 120.1 . . ?
C9 C10 H10 119.3 . . ?
C9 C10 C11 121.5(2) . . ?
C11 C10 H10 119.3 . . ?
C73 C72 H72 120.1 . . ?
C73 C72 C71 119.7(2) . . ?
C71 C72 H72 120.1 . . ?
C69 C70 C75 122.03(18) . . ?
C71 C70 C69 118.5(2) . . ?
C71 C70 C75 119.4(2) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C10 C9 H9 120.0 . . ?
C10 C9 C8 120.0(2) . . ?
C8 C9 H9 120.0 . . ?
C19 C24 H24 108.0 . . ?
C19 C24 C25 109.59(18) . . ?
C19 C24 C26 112.60(18) . . ?
C25 C24 H24 108.0 . . ?
C25 C24 C26 110.63(19) . . ?
C26 C24 H24 108.0 . . ?
C20 C19 C24 118.8(2) . . ?
C20 C19 C18 118.3(2) . . ?
C18 C19 C24 122.68(18) . . ?
C18 C23 C27 122.84(19) . . ?
C22 C23 C27 118.7(2) . . ?
C22 C23 C18 118.5(2) . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C40 C41 H41 119.1 . . ?
C42 C41 C40 121.7(2) . . ?
C42 C41 H41 119.1 . . ?
C19 C20 H20 119.2 . . ?
C21 C20 C19 121.6(2) . . ?
C21 C20 H20 119.2 . . ?
C19 C18 N2 118.38(18) . . ?
C19 C18 C23 120.77(19) . . ?
C23 C18 N2 120.74(19) . . ?
C52 C55 H55A 109.5 . . ?
C52 C55 H55B 109.5 . . ?
C52 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C74 C73 H73 119.4 . . ?
C72 C73 C74 121.3(2) . . ?
C72 C73 H73 119.4 . . ?
C97 C102 H102 119.5 . . ?
C101 C102 C97 121.0(2) . . ?
C101 C102 H102 119.5 . . ?
C58 C59 H59 119.3 . . ?
C60 C59 C58 121.5(2) . . ?
C60 C59 H59 119.3 . . ?
C7 C8 H8 119.3 . . ?
C9 C8 C7 121.4(2) . . ?
C9 C8 H8 119.3 . . ?
C20 C21 H21 120.5 . . ?
C22 C21 C20 119.1(2) . . ?
C22 C21 H21 120.5 . . ?
N3 C30 C33 111.30(18) . . ?
N3 C30 C32 108.96(17) . . ?
N3 C30 C31 108.77(18) . . ?
C33 C30 C32 109.18(19) . . ?
C33 C30 C31 109.40(19) . . ?
C31 C30 C32 109.2(2) . . ?
C23 C22 H22 119.2 . . ?
C21 C22 C23 121.6(2) . . ?
C21 C22 H22 119.2 . . ?
C72 C71 C70 121.1(2) . . ?
C72 C71 H71 119.5 . . ?
C70 C71 H71 119.5 . . ?
C7 C12 H12 108.1 . . ?
C7 C12 C13 112.22(19) . . ?
C7 C12 C14 111.7(2) . . ?
C13 C12 H12 108.1 . . ?
C14 C12 H12 108.1 . . ?
C14 C12 C13 108.4(2) . . ?
C74 C78 H78 108.0 . . ?
C74 C78 C79 111.82(19) . . ?
C74 C78 C80 109.97(19) . . ?
C79 C78 H78 108.0 . . ?
C80 C78 H78 108.0 . . ?
C80 C78 C79 110.9(2) . . ?
C41 C42 H42 119.9 . . ?
C41 C42 C43 120.1(2) . . ?
C43 C42 H42 119.9 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N7 C81 C83 111.22(18) . . ?
N7 C81 C84 108.40(18) . . ?
N7 C81 C82 109.50(17) . . ?
C83 C81 C84 109.70(19) . . ?
C83 C81 C82 109.51(19) . . ?
C84 C81 C82 108.46(19) . . ?
C101 C100 H100 120.3 . . ?
C99 C100 H100 120.3 . . ?
C99 C100 C101 119.4(2) . . ?
N8 C85 C87 111.92(18) . . ?
N8 C85 C88 111.23(18) . . ?
N8 C85 C86 107.11(17) . . ?
C88 C85 C87 109.99(19) . . ?
C88 C85 C86 108.6(2) . . ?
C86 C85 C87 107.87(19) . . ?
C91 C96 H96 119.5 . . ?
C95 C96 C91 121.0(2) . . ?
C95 C96 H96 119.5 . . ?
C96 C95 H95 119.6 . . ?
C94 C95 C96 120.7(2) . . ?
C94 C95 H95 119.6 . . ?
C93 C94 H94 120.4 . . ?
C95 C94 C93 119.3(2) . . ?
C95 C94 H94 120.4 . . ?
C85 C87 H87A 109.5 . . ?
C85 C87 H87B 109.5 . . ?
C85 C87 H87C 109.5 . . ?
H87A C87 H87B 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C50 C49 H49 120.4 . . ?
C48 C49 H49 120.4 . . ?
C48 C49 C50 119.2(2) . . ?
C6 C11 C15 122.9(2) . . ?
C10 C11 C6 117.8(2) . . ?
C10 C11 C15 119.2(2) . . ?
C51 C50 C49 120.8(2) . . ?
C51 C50 H50 119.6 . . ?
C49 C50 H50 119.6 . . ?
C42 C43 H43 120.5 . . ?
C44 C43 C42 119.1(2) . . ?
C44 C43 H43 120.5 . . ?
C102 C101 C100 120.5(2) . . ?
C102 C101 H101 119.7 . . ?
C100 C101 H101 119.7 . . ?
C97 C98 H98 119.4 . . ?
C99 C98 C97 121.2(2) . . ?
C99 C98 H98 119.4 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
C100 C99 C98 120.3(2) . . ?
C100 C99 H99 119.9 . . ?
C98 C99 H99 119.9 . . ?
C40 C45 H45 119.3 . . ?
C44 C45 C40 121.3(2) . . ?
C44 C45 H45 119.3 . . ?
C85 C88 H88A 109.5 . . ?
C85 C88 H88B 109.5 . . ?
C85 C88 H88C 109.5 . . ?
H88A C88 H88B 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C49 C48 H48 119.9 . . ?
C49 C48 C47 120.2(2) . . ?
C47 C48 H48 119.9 . . ?
N4 C34 C36 111.41(18) . . ?
N4 C34 C37 111.75(18) . . ?
N4 C34 C35 107.20(17) . . ?
C37 C34 C36 109.73(19) . . ?
C37 C34 C35 107.4(2) . . ?
C35 C34 C36 109.21(19) . . ?
C81 C83 H83A 109.5 . . ?
C81 C83 H83B 109.5 . . ?
C81 C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C62 C66 H66 108.2 . . ?
C62 C66 C67 112.25(19) . . ?
C62 C66 C68 109.6(2) . . ?
C67 C66 H66 108.2 . . ?
C68 C66 H66 108.2 . . ?
C68 C66 C67 110.2(2) . . ?
C46 C47 H47 119.4 . . ?
C48 C47 C46 121.2(2) . . ?
C48 C47 H47 119.4 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C75 C77 H77A 109.5 . . ?
C75 C77 H77B 109.5 . . ?
C75 C77 H77C 109.5 . . ?
H77A C77 H77B 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C43 C44 C45 120.7(2) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 H44 119.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C11 C15 H15 107.1 . . ?
C11 C15 C17 112.6(2) . . ?
C17 C15 H15 107.1 . . ?
C16 C15 C11 111.9(2) . . ?
C16 C15 H15 107.1 . . ?
C16 C15 C17 110.8(2) . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C81 C84 H84A 109.5 . . ?
C81 C84 H84B 109.5 . . ?
C81 C84 H84C 109.5 . . ?
H84A C84 H84B 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C85 C86 H86A 109.5 . . ?
C85 C86 H86B 109.5 . . ?
C85 C86 H86C 109.5 . . ?
H86A C86 H86B 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C78 C79 H79A 109.5 . . ?
C78 C79 H79B 109.5 . . ?
C78 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76B 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C66 C68 H68A 109.5 . . ?
C66 C68 H68B 109.5 . . ?
C66 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C78 C80 H80A 109.5 . . ?
C78 C80 H80B 109.5 . . ?
C78 C80 H80C 109.5 . . ?
H80A C80 H80B 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bmkxr72
_database_code_depnum_ccdc_archive 'CCDC 2004176'
loop_
_audit_author_name
_audit_author_address
'Jade Fostvedt'
;UC Berkeley College of Chemistry
United States of America
;
_audit_update_record             
;
2020-05-15 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_bmkxr72             
;
PROBLEM: Check Calcd Positive Resid. Density on       Nb1       1.63 eA-3  
RESPONSE: Possible minor unresolved twinning or disorder near a heavy atom. 
;
# end Validation Reply Form
_audit_creation_date             2020-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            (κ1-BDI)Nb(Py)(NAr)-(μ-O)2-(NAr)Nb(BDI)
_chemical_name_systematic        
'bis(μ2-oxido)-bis(2,6-diisopropylphenyl)imino-(N-(4-((2,6-diisopropylphenyl)imino)pent-2-en-2-yl)-2,6-diisopropylanilido)-pyridine-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-diniobium(V) diethyl ether solvate'
_chemical_formula_moiety         'C87 H121 N7 Nb2 O2, C4 H10 O'
_chemical_formula_sum            'C91 H131 N7 Nb2 O3'
_chemical_formula_weight         1556.84
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.6394(12)
_cell_length_b                   20.8107(13)
_cell_length_c                   25.0878(15)
_cell_angle_alpha                90
_cell_angle_beta                 100.6670(10)
_cell_angle_gamma                90
_cell_volume                     9050.3(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.29
_shelx_estimated_absorpt_T_max   0.970
_shelx_estimated_absorpt_T_min   0.948
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6621
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0497 before and 0.0413 after correction.
The Ratio of minimum to maximum transmission is 0.8885.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            83162
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.359
_diffrn_reflns_theta_min         1.280
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12436
_reflns_number_total             16411
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         16411
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0445
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0729P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1237
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C36(H36), C39(H39), C53(H53),
 C56(H56), C65(H65), C68(H68), C77(H77), C80(H80)
2.b Secondary CH2 refined with riding coordinates:
 C89(H89A,H89B), C90(H90A,H90B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32),
 C33(H33), C34(H34), C43(H43), C49(H49), C50(H50), C51(H51), C61(H61), C62(H62),
  C63(H63), C73(H73), C74(H74), C75(H75), C83(H83), C84(H84), C85(H85),
 C86(H86), C87(H87)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C69(H69A,
 H69B,H69C), C70(H70A,H70B,H70C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C),
 C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C88(H88A,H88B,H88C), C91(H91A,H91B,
 H91C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.46108(15) 0.19246(12) 0.02562(11) 0.0181(6) Uani 1 1 d . . . . .
C2 C 0.45547(16) 0.25291(12) 0.00065(12) 0.0194(6) Uani 1 1 d . . . . .
H2 H 0.439755 0.252796 -0.037674 0.023 Uiso 1 1 calc R . . . .
C3 C 0.46989(15) 0.31332(12) 0.02460(11) 0.0177(6) Uani 1 1 d . . . . .
C4 C 0.43202(17) 0.13630(12) -0.01124(11) 0.0241(7) Uani 1 1 d . . . . .
H4A H 0.475347 0.108092 -0.014658 0.036 Uiso 1 1 calc GR . . . .
H4B H 0.408270 0.152503 -0.047133 0.036 Uiso 1 1 calc GR . . . .
H4C H 0.393695 0.112090 0.004297 0.036 Uiso 1 1 calc GR . . . .
C5 C 0.44933(17) 0.37024(12) -0.01308(12) 0.0241(7) Uani 1 1 d . . . . .
H5A H 0.415867 0.399697 0.002420 0.036 Uiso 1 1 calc GR . . . .
H5B H 0.422262 0.355051 -0.048497 0.036 Uiso 1 1 calc GR . . . .
H5C H 0.496581 0.392738 -0.017498 0.036 Uiso 1 1 calc GR . . . .
C6 C 0.47880(16) 0.11791(12) 0.09771(11) 0.0207(6) Uani 1 1 d . . . . .
C7 C 0.53340(17) 0.06898(12) 0.09393(11) 0.0222(6) Uani 1 1 d . . . . .
C8 C 0.51392(18) 0.00643(13) 0.10661(12) 0.0255(7) Uani 1 1 d . . . . .
H8 H 0.549375 -0.027391 0.104386 0.031 Uiso 1 1 calc R . . . .
C9 C 0.44524(18) -0.00762(13) 0.12215(12) 0.0288(7) Uani 1 1 d . . . . .
H9 H 0.433098 -0.050743 0.129740 0.035 Uiso 1 1 calc R . . . .
C10 C 0.39372(18) 0.04128(13) 0.12674(12) 0.0263(7) Uani 1 1 d . . . . .
H10 H 0.346458 0.031353 0.137905 0.032 Uiso 1 1 calc R . . . .
C11 C 0.40981(16) 0.10477(12) 0.11529(11) 0.0211(6) Uani 1 1 d . . . . .
C12 C 0.61011(17) 0.08195(12) 0.07691(12) 0.0232(6) Uani 1 1 d . . . . .
H12 H 0.608290 0.126162 0.061113 0.028 Uiso 1 1 calc R . . . .
C13 C 0.62821(18) 0.03429(13) 0.03394(12) 0.0290(7) Uani 1 1 d . . . . .
H13A H 0.638539 -0.008268 0.050399 0.044 Uiso 1 1 calc GR . . . .
H13B H 0.673633 0.049134 0.020127 0.044 Uiso 1 1 calc GR . . . .
H13C H 0.583949 0.031710 0.003968 0.044 Uiso 1 1 calc GR . . . .
C14 C 0.67499(17) 0.08023(13) 0.12708(12) 0.0275(7) Uani 1 1 d . . . . .
H14A H 0.664503 0.112134 0.153523 0.041 Uiso 1 1 calc GR . . . .
H14B H 0.724322 0.090137 0.116279 0.041 Uiso 1 1 calc GR . . . .
H14C H 0.677524 0.037340 0.143436 0.041 Uiso 1 1 calc GR . . . .
C15 C 0.35067(16) 0.15729(13) 0.11993(11) 0.0230(6) Uani 1 1 d . . . . .
H15 H 0.378869 0.199193 0.124574 0.028 Uiso 1 1 calc R . . . .
C16 C 0.28856(18) 0.16235(16) 0.06846(13) 0.0377(8) Uani 1 1 d . . . . .
H16A H 0.312188 0.177068 0.038211 0.057 Uiso 1 1 calc GR . . . .
H16B H 0.248933 0.193102 0.074497 0.057 Uiso 1 1 calc GR . . . .
H16C H 0.264906 0.120112 0.059799 0.057 Uiso 1 1 calc GR . . . .
C17 C 0.31179(17) 0.14816(14) 0.16939(12) 0.0290(7) Uani 1 1 d . . . . .
H17A H 0.276348 0.111523 0.163116 0.043 Uiso 1 1 calc GR . . . .
H17B H 0.282948 0.187080 0.174929 0.043 Uiso 1 1 calc GR . . . .
H17C H 0.351270 0.140047 0.201664 0.043 Uiso 1 1 calc GR . . . .
C18 C 0.49552(16) 0.38850(12) 0.09605(11) 0.0190(6) Uani 1 1 d . . . . .
C19 C 0.42786(16) 0.40783(13) 0.11363(12) 0.0229(6) Uani 1 1 d . . . . .
C20 C 0.42214(18) 0.47213(13) 0.12796(12) 0.0285(7) Uani 1 1 d . . . . .
H20 H 0.376605 0.486499 0.139410 0.034 Uiso 1 1 calc R . . . .
C21 C 0.48087(18) 0.51562(13) 0.12599(12) 0.0298(7) Uani 1 1 d . . . . .
H21 H 0.475449 0.559223 0.135866 0.036 Uiso 1 1 calc R . . . .
C22 C 0.54707(18) 0.49533(13) 0.10967(12) 0.0276(7) Uani 1 1 d . . . . .
H22 H 0.587480 0.525269 0.108812 0.033 Uiso 1 1 calc R . . . .
C23 C 0.55642(16) 0.43152(12) 0.09425(11) 0.0217(6) Uani 1 1 d . . . . .
C24 C 0.36173(16) 0.36193(13) 0.11616(12) 0.0258(7) Uani 1 1 d . . . . .
H24 H 0.384607 0.318510 0.125608 0.031 Uiso 1 1 calc R . . . .
C25 C 0.30480(18) 0.35547(16) 0.06190(13) 0.0356(8) Uani 1 1 d . . . . .
H25A H 0.287263 0.398250 0.048672 0.053 Uiso 1 1 calc GR . . . .
H25B H 0.260339 0.329696 0.067286 0.053 Uiso 1 1 calc GR . . . .
H25C H 0.330600 0.334364 0.035232 0.053 Uiso 1 1 calc GR . . . .
C26 C 0.31580(18) 0.38036(15) 0.16020(13) 0.0342(8) Uani 1 1 d . . . . .
H26A H 0.351583 0.391741 0.193588 0.051 Uiso 1 1 calc GR . . . .
H26B H 0.283913 0.343892 0.167247 0.051 Uiso 1 1 calc GR . . . .
H26C H 0.282570 0.417222 0.147886 0.051 Uiso 1 1 calc GR . . . .
C27 C 0.63039(17) 0.41315(12) 0.07527(12) 0.0248(7) Uani 1 1 d . . . . .
H27 H 0.624575 0.367791 0.061987 0.030 Uiso 1 1 calc R . . . .
C28 C 0.64590(19) 0.45514(13) 0.02797(13) 0.0311(7) Uani 1 1 d . . . . .
H28A H 0.600233 0.455175 -0.000998 0.047 Uiso 1 1 calc GR . . . .
H28B H 0.690038 0.437796 0.013995 0.047 Uiso 1 1 calc GR . . . .
H28C H 0.657314 0.499190 0.040788 0.047 Uiso 1 1 calc GR . . . .
C29 C 0.70007(18) 0.41532(14) 0.12223(13) 0.0313(7) Uani 1 1 d . . . . .
H29A H 0.704508 0.458399 0.138279 0.047 Uiso 1 1 calc GR . . . .
H29B H 0.747175 0.405176 0.108465 0.047 Uiso 1 1 calc GR . . . .
H29C H 0.692934 0.383759 0.149871 0.047 Uiso 1 1 calc GR . . . .
C30 C 0.72066(16) 0.22444(12) 0.07135(12) 0.0224(6) Uani 1 1 d . . . . .
C31 C 0.71027(16) 0.21648(14) 0.01424(12) 0.0253(7) Uani 1 1 d . . . . .
C32 C 0.77314(19) 0.19984(17) -0.00932(14) 0.0395(8) Uani 1 1 d . . . . .
H32 H 0.766012 0.194492 -0.047526 0.047 Uiso 1 1 calc R . . . .
C33 C 0.8456(2) 0.19096(19) 0.02176(15) 0.0477(10) Uani 1 1 d . . . . .
H33 H 0.887966 0.179963 0.005068 0.057 Uiso 1 1 calc R . . . .
C34 C 0.85577(19) 0.19821(17) 0.07710(14) 0.0407(9) Uani 1 1 d . . . . .
H34 H 0.905766 0.192310 0.098314 0.049 Uiso 1 1 calc R . . . .
C35 C 0.79496(17) 0.21392(15) 0.10288(12) 0.0283(7) Uani 1 1 d . . . . .
C36 C 0.63290(17) 0.22800(14) -0.02195(12) 0.0254(7) Uani 1 1 d . . . . .
H36 H 0.592778 0.225182 0.001367 0.031 Uiso 1 1 calc R . . . .
C37 C 0.62857(18) 0.29592(14) -0.04623(13) 0.0306(7) Uani 1 1 d . . . . .
H37A H 0.636471 0.327683 -0.016886 0.046 Uiso 1 1 calc GR . . . .
H37B H 0.577761 0.302471 -0.069093 0.046 Uiso 1 1 calc GR . . . .
H37C H 0.668694 0.300947 -0.068204 0.046 Uiso 1 1 calc GR . . . .
C38 C 0.61213(19) 0.17802(14) -0.06743(13) 0.0325(8) Uani 1 1 d . . . . .
H38A H 0.644620 0.184622 -0.094699 0.049 Uiso 1 1 calc GR . . . .
H38B H 0.557761 0.182851 -0.084439 0.049 Uiso 1 1 calc GR . . . .
H38C H 0.620763 0.134722 -0.052153 0.049 Uiso 1 1 calc GR . . . .
C39 C 0.81113(17) 0.22144(15) 0.16442(12) 0.0297(7) Uani 1 1 d . . . . .
H39 H 0.760870 0.219885 0.177401 0.036 Uiso 1 1 calc R . . . .
C40 C 0.86314(19) 0.16827(15) 0.19295(13) 0.0364(8) Uani 1 1 d . . . . .
H40A H 0.913307 0.169951 0.181524 0.055 Uiso 1 1 calc GR . . . .
H40B H 0.839062 0.126385 0.183324 0.055 Uiso 1 1 calc GR . . . .
H40C H 0.870405 0.174364 0.232305 0.055 Uiso 1 1 calc GR . . . .
C41 C 0.8483(2) 0.28616(16) 0.17958(15) 0.0460(9) Uani 1 1 d . . . . .
H41A H 0.861493 0.289785 0.219157 0.069 Uiso 1 1 calc GR . . . .
H41B H 0.812151 0.320456 0.165202 0.069 Uiso 1 1 calc GR . . . .
H41C H 0.895230 0.290112 0.164171 0.069 Uiso 1 1 calc GR . . . .
C42 C 0.44796(16) 0.23576(12) 0.28817(12) 0.0196(6) Uani 1 1 d . . . . .
C43 C 0.39711(16) 0.21989(12) 0.32093(12) 0.0220(6) Uani 1 1 d . . . . .
H43 H 0.417740 0.195461 0.352250 0.026 Uiso 1 1 calc R . . . .
C44 C 0.31499(17) 0.23553(13) 0.31420(13) 0.0239(7) Uani 1 1 d . . . . .
C45 C 0.42341(16) 0.26541(13) 0.23274(12) 0.0215(6) Uani 1 1 d . . . . .
H45A H 0.367151 0.270019 0.224840 0.032 Uiso 1 1 calc GR . . . .
H45B H 0.439698 0.237665 0.205366 0.032 Uiso 1 1 calc GR . . . .
H45C H 0.447434 0.307782 0.232017 0.032 Uiso 1 1 calc GR . . . .
C46 C 0.27822(18) 0.21156(15) 0.36061(13) 0.0349(8) Uani 1 1 d . . . . .
H46A H 0.227817 0.232120 0.358777 0.052 Uiso 1 1 calc GR . . . .
H46B H 0.311577 0.222230 0.395218 0.052 Uiso 1 1 calc GR . . . .
H46C H 0.271515 0.164861 0.357783 0.052 Uiso 1 1 calc GR . . . .
C47 C 0.55056(16) 0.18101(12) 0.34722(12) 0.0209(6) Uani 1 1 d . . . . .
C48 C 0.53287(16) 0.11513(13) 0.33853(12) 0.0243(7) Uani 1 1 d . . . . .
C49 C 0.54723(17) 0.07393(14) 0.38305(13) 0.0297(7) Uani 1 1 d . . . . .
H49 H 0.536130 0.029464 0.377788 0.036 Uiso 1 1 calc R . . . .
C50 C 0.57725(18) 0.09598(14) 0.43482(13) 0.0332(8) Uani 1 1 d . . . . .
H50 H 0.584806 0.067372 0.464843 0.040 Uiso 1 1 calc R . . . .
C51 C 0.59593(18) 0.16002(14) 0.44197(13) 0.0316(7) Uani 1 1 d . . . . .
H51 H 0.617212 0.175082 0.477326 0.038 Uiso 1 1 calc R . . . .
C52 C 0.58457(17) 0.20341(13) 0.39894(12) 0.0247(7) Uani 1 1 d . . . . .
C53 C 0.49723(16) 0.08776(13) 0.28370(12) 0.0251(7) Uani 1 1 d . . . . .
H53 H 0.484573 0.124595 0.258004 0.030 Uiso 1 1 calc R . . . .
C54 C 0.55390(19) 0.04411(15) 0.26147(14) 0.0366(8) Uani 1 1 d . . . . .
H54A H 0.598541 0.069367 0.255628 0.055 Uiso 1 1 calc GR . . . .
H54B H 0.528315 0.025336 0.226980 0.055 Uiso 1 1 calc GR . . . .
H54C H 0.571139 0.009685 0.287554 0.055 Uiso 1 1 calc GR . . . .
C55 C 0.42212(18) 0.05195(14) 0.28566(14) 0.0354(8) Uani 1 1 d . . . . .
H55A H 0.433486 0.012924 0.307543 0.053 Uiso 1 1 calc GR . . . .
H55B H 0.397031 0.040254 0.248756 0.053 Uiso 1 1 calc GR . . . .
H55C H 0.387706 0.079702 0.301918 0.053 Uiso 1 1 calc GR . . . .
C56 C 0.60639(19) 0.27311(14) 0.41035(13) 0.0304(7) Uani 1 1 d . . . . .
H56 H 0.602713 0.295431 0.374664 0.036 Uiso 1 1 calc R . . . .
C57 C 0.6898(2) 0.28017(16) 0.44119(14) 0.0476(10) Uani 1 1 d . . . . .
H57A H 0.695474 0.257767 0.476068 0.071 Uiso 1 1 calc GR . . . .
H57B H 0.701919 0.325811 0.447523 0.071 Uiso 1 1 calc GR . . . .
H57C H 0.725280 0.261421 0.419650 0.071 Uiso 1 1 calc GR . . . .
C58 C 0.5499(2) 0.30592(16) 0.44109(14) 0.0476(10) Uani 1 1 d . . . . .
H58A H 0.497246 0.301261 0.420549 0.071 Uiso 1 1 calc GR . . . .
H58B H 0.562759 0.351650 0.445595 0.071 Uiso 1 1 calc GR . . . .
H58C H 0.553494 0.285878 0.476816 0.071 Uiso 1 1 calc GR . . . .
C59 C 0.20261(16) 0.29068(14) 0.27170(12) 0.0262(7) Uani 1 1 d . . . . .
C60 C 0.19549(17) 0.35752(14) 0.28086(12) 0.0267(7) Uani 1 1 d . . . . .
C61 C 0.12191(19) 0.38374(15) 0.27609(13) 0.0340(8) Uani 1 1 d . . . . .
H61 H 0.116427 0.428353 0.282436 0.041 Uiso 1 1 calc R . . . .
C62 C 0.05711(19) 0.34628(16) 0.26238(14) 0.0372(8) Uani 1 1 d . . . . .
H62 H 0.007402 0.365040 0.259401 0.045 Uiso 1 1 calc R . . . .
C63 C 0.06415(18) 0.28148(16) 0.25293(14) 0.0357(8) Uani 1 1 d . . . . .
H63 H 0.018910 0.256109 0.243310 0.043 Uiso 1 1 calc R . . . .
C64 C 0.13624(18) 0.25235(14) 0.25720(14) 0.0291(7) Uani 1 1 d . . . . .
C65 C 0.26844(17) 0.39791(13) 0.29788(13) 0.0285(7) Uani 1 1 d . . . . .
H65 H 0.310631 0.376624 0.282699 0.034 Uiso 1 1 calc R . . . .
C66 C 0.2928(2) 0.39821(16) 0.35949(14) 0.0396(8) Uani 1 1 d . . . . .
H66A H 0.251155 0.416123 0.375868 0.059 Uiso 1 1 calc GR . . . .
H66B H 0.339308 0.424559 0.369732 0.059 Uiso 1 1 calc GR . . . .
H66C H 0.303750 0.354147 0.372449 0.059 Uiso 1 1 calc GR . . . .
C67 C 0.26102(19) 0.46658(14) 0.27595(14) 0.0387(8) Uani 1 1 d . . . . .
H67A H 0.240568 0.465677 0.236876 0.058 Uiso 1 1 calc GR . . . .
H67B H 0.311864 0.487166 0.282549 0.058 Uiso 1 1 calc GR . . . .
H67C H 0.225871 0.490925 0.294355 0.058 Uiso 1 1 calc GR . . . .
C68 C 0.14125(18) 0.18104(15) 0.24405(14) 0.0346(8) Uani 1 1 d . . . . .
H68 H 0.196954 0.168556 0.251228 0.042 Uiso 1 1 calc R . . . .
C69 C 0.0995(2) 0.13911(16) 0.28005(16) 0.0479(10) Uani 1 1 d . . . . .
H69A H 0.120778 0.147748 0.318299 0.072 Uiso 1 1 calc GR . . . .
H69B H 0.106933 0.093657 0.272177 0.072 Uiso 1 1 calc GR . . . .
H69C H 0.044320 0.149211 0.272618 0.072 Uiso 1 1 calc GR . . . .
C70 C 0.1089(2) 0.16829(18) 0.18417(15) 0.0480(10) Uani 1 1 d . . . . .
H70A H 0.053243 0.176701 0.176798 0.072 Uiso 1 1 calc GR . . . .
H70B H 0.118274 0.123373 0.175609 0.072 Uiso 1 1 calc GR . . . .
H70C H 0.134321 0.196604 0.161698 0.072 Uiso 1 1 calc GR . . . .
C71 C 0.76675(16) 0.25169(12) 0.30768(12) 0.0189(6) Uani 1 1 d . . . . .
C72 C 0.79800(16) 0.19111(12) 0.32478(11) 0.0217(6) Uani 1 1 d . . . . .
C73 C 0.87770(16) 0.18640(13) 0.34307(11) 0.0230(6) Uani 1 1 d . . . . .
H73 H 0.899807 0.145637 0.353502 0.028 Uiso 1 1 calc R . . . .
C74 C 0.92479(17) 0.23960(13) 0.34627(12) 0.0238(7) Uani 1 1 d . . . . .
H74 H 0.978930 0.235183 0.357897 0.029 Uiso 1 1 calc R . . . .
C75 C 0.89289(16) 0.29971(13) 0.33246(12) 0.0247(7) Uani 1 1 d . . . . .
H75 H 0.925421 0.336453 0.336685 0.030 Uiso 1 1 calc R . . . .
C76 C 0.81432(16) 0.30734(12) 0.31256(11) 0.0205(6) Uani 1 1 d . . . . .
C77 C 0.74693(16) 0.13239(13) 0.32496(12) 0.0258(7) Uani 1 1 d . . . . .
H77 H 0.692280 0.145891 0.311698 0.031 Uiso 1 1 calc R . . . .
C78 C 0.76678(19) 0.08039(14) 0.28676(13) 0.0357(8) Uani 1 1 d . . . . .
H78A H 0.757764 0.096905 0.249540 0.054 Uiso 1 1 calc GR . . . .
H78B H 0.734172 0.042627 0.288614 0.054 Uiso 1 1 calc GR . . . .
H78C H 0.821139 0.068282 0.297635 0.054 Uiso 1 1 calc GR . . . .
C79 C 0.75292(18) 0.10618(14) 0.38229(13) 0.0333(8) Uani 1 1 d . . . . .
H79A H 0.805728 0.091354 0.395739 0.050 Uiso 1 1 calc GR . . . .
H79B H 0.717044 0.070160 0.381925 0.050 Uiso 1 1 calc GR . . . .
H79C H 0.739848 0.140167 0.406070 0.050 Uiso 1 1 calc GR . . . .
C80 C 0.77918(16) 0.37283(12) 0.29728(12) 0.0250(7) Uani 1 1 d . . . . .
H80 H 0.734865 0.366418 0.266560 0.030 Uiso 1 1 calc R . . . .
C81 C 0.83459(18) 0.42055(13) 0.27826(13) 0.0312(7) Uani 1 1 d . . . . .
H81A H 0.878424 0.428430 0.307757 0.047 Uiso 1 1 calc GR . . . .
H81B H 0.807547 0.461070 0.267913 0.047 Uiso 1 1 calc GR . . . .
H81C H 0.853295 0.402696 0.246937 0.047 Uiso 1 1 calc GR . . . .
C82 C 0.74662(18) 0.40036(13) 0.34498(13) 0.0303(7) Uani 1 1 d . . . . .
H82A H 0.708380 0.370564 0.354726 0.045 Uiso 1 1 calc GR . . . .
H82B H 0.722054 0.441876 0.334584 0.045 Uiso 1 1 calc GR . . . .
H82C H 0.788588 0.406263 0.376152 0.045 Uiso 1 1 calc GR . . . .
C83 C 0.58179(16) 0.42145(13) 0.25034(12) 0.0245(7) Uani 1 1 d . . . . .
H83 H 0.608339 0.415187 0.221079 0.029 Uiso 1 1 calc R . . . .
C84 C 0.56702(17) 0.48338(13) 0.26517(13) 0.0284(7) Uani 1 1 d . . . . .
H84 H 0.583859 0.518842 0.246549 0.034 Uiso 1 1 calc R . . . .
C85 C 0.52785(19) 0.49365(14) 0.30699(13) 0.0332(8) Uani 1 1 d . . . . .
H85 H 0.517560 0.536056 0.317721 0.040 Uiso 1 1 calc R . . . .
C86 C 0.50381(18) 0.44117(14) 0.33303(13) 0.0323(7) Uani 1 1 d . . . . .
H86 H 0.476537 0.446735 0.361997 0.039 Uiso 1 1 calc R . . . .
C87 C 0.52018(17) 0.38024(13) 0.31616(12) 0.0255(7) Uani 1 1 d . . . . .
H87 H 0.502583 0.344302 0.333804 0.031 Uiso 1 1 calc R . . . .
C88 C 0.5966(5) 0.1279(5) 0.6172(3) 0.206(5) Uani 1 1 d . . . . .
H88A H 0.614720 0.086022 0.606903 0.310 Uiso 1 1 calc GR . . . .
H88B H 0.611473 0.133583 0.656556 0.310 Uiso 1 1 calc GR . . . .
H88C H 0.619859 0.162049 0.598673 0.310 Uiso 1 1 calc GR . . . .
C89 C 0.5121(5) 0.1311(4) 0.6016(4) 0.163(3) Uani 1 1 d . . . . .
H89A H 0.489916 0.106812 0.628929 0.196 Uiso 1 1 calc R . . . .
H89B H 0.496667 0.176547 0.604105 0.196 Uiso 1 1 calc R . . . .
C90 C 0.4072(5) 0.1050(5) 0.5295(5) 0.219(6) Uani 1 1 d . . . . .
H90A H 0.385590 0.148018 0.534465 0.263 Uiso 1 1 calc R . . . .
H90B H 0.384252 0.075701 0.553323 0.263 Uiso 1 1 calc R . . . .
C91 C 0.3731(5) 0.0867(5) 0.4763(3) 0.187(5) Uani 1 1 d . . . . .
H91A H 0.396136 0.111677 0.450185 0.281 Uiso 1 1 calc GR . . . .
H91B H 0.317511 0.095007 0.470391 0.281 Uiso 1 1 calc GR . . . .
H91C H 0.382123 0.040844 0.471228 0.281 Uiso 1 1 calc GR . . . .
N1 N 0.49143(12) 0.18248(9) 0.07793(9) 0.0164(5) Uani 1 1 d . . . . .
N2 N 0.50053(13) 0.32252(10) 0.07689(9) 0.0179(5) Uani 1 1 d . . . . .
N3 N 0.65723(13) 0.23994(10) 0.09526(10) 0.0178(5) Uani 1 1 d . . . . .
N4 N 0.52719(13) 0.22455(10) 0.30164(9) 0.0192(5) Uani 1 1 d . . . . .
N5 N 0.27873(13) 0.26734(11) 0.27403(10) 0.0238(5) Uani 1 1 d . . . . .
N6 N 0.68800(13) 0.25755(9) 0.28607(10) 0.0176(5) Uani 1 1 d . . . . .
N7 N 0.55984(13) 0.36925(10) 0.27593(9) 0.0202(5) Uani 1 1 d . . . . .
O1 O 0.59003(10) 0.31627(8) 0.18172(7) 0.0185(4) Uani 1 1 d . . . . .
O2 O 0.57857(10) 0.19700(8) 0.19112(7) 0.0179(4) Uani 1 1 d . . . . .
O3 O 0.4784(3) 0.1090(3) 0.5517(2) 0.148(2) Uani 1 1 d . . . . .
Nb1 Nb 0.57413(2) 0.24993(2) 0.12654(2) 0.01526(8) Uani 1 1 d . . . . .
Nb2 Nb 0.59281(2) 0.26363(2) 0.24778(2) 0.01624(8) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.401(3) . ?
C1 C4 1.519(3) . ?
C1 N1 1.339(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.396(4) . ?
C3 C5 1.517(4) . ?
C3 N2 1.337(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.417(4) . ?
C6 C11 1.396(4) . ?
C6 N1 1.464(3) . ?
C7 C8 1.398(4) . ?
C7 C12 1.517(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.371(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.383(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.393(4) . ?
C11 C15 1.530(4) . ?
C12 H12 1.0000 . ?
C12 C13 1.541(4) . ?
C12 C14 1.537(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.535(4) . ?
C15 C17 1.537(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.406(4) . ?
C18 C23 1.406(4) . ?
C18 N2 1.463(3) . ?
C19 C20 1.394(4) . ?
C19 C24 1.518(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.383(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.374(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.401(4) . ?
C23 C27 1.518(4) . ?
C24 H24 1.0000 . ?
C24 C25 1.541(4) . ?
C24 C26 1.535(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27 1.0000 . ?
C27 C28 1.538(4) . ?
C27 C29 1.538(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.420(4) . ?
C30 C35 1.417(4) . ?
C30 N3 1.401(4) . ?
C31 C32 1.393(4) . ?
C31 C36 1.512(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.381(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.375(5) . ?
C34 H34 0.9500 . ?
C34 C35 1.390(4) . ?
C35 C39 1.525(4) . ?
C36 H36 1.0000 . ?
C36 C37 1.535(4) . ?
C36 C38 1.537(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39 1.0000 . ?
C39 C40 1.528(4) . ?
C39 C41 1.515(5) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.365(4) . ?
C42 C45 1.510(4) . ?
C42 N4 1.395(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.464(4) . ?
C44 C46 1.518(4) . ?
C44 N5 1.274(4) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.414(4) . ?
C47 C52 1.404(4) . ?
C47 N4 1.457(3) . ?
C48 C49 1.394(4) . ?
C48 C53 1.514(4) . ?
C49 H49 0.9500 . ?
C49 C50 1.387(4) . ?
C50 H50 0.9500 . ?
C50 C51 1.377(4) . ?
C51 H51 0.9500 . ?
C51 C52 1.393(4) . ?
C52 C56 1.514(4) . ?
C53 H53 1.0000 . ?
C53 C54 1.530(4) . ?
C53 C55 1.529(4) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56 1.0000 . ?
C56 C57 1.538(5) . ?
C56 C58 1.529(4) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C60 1.419(4) . ?
C59 C64 1.408(4) . ?
C59 N5 1.419(4) . ?
C60 C61 1.392(4) . ?
C60 C65 1.530(4) . ?
C61 H61 0.9500 . ?
C61 C62 1.374(4) . ?
C62 H62 0.9500 . ?
C62 C63 1.379(4) . ?
C63 H63 0.9500 . ?
C63 C64 1.395(4) . ?
C64 C68 1.526(4) . ?
C65 H65 1.0000 . ?
C65 C66 1.526(4) . ?
C65 C67 1.528(4) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68 1.0000 . ?
C68 C69 1.538(4) . ?
C68 C70 1.528(5) . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 C72 1.411(4) . ?
C71 C76 1.422(4) . ?
C71 N6 1.400(4) . ?
C72 C73 1.399(4) . ?
C72 C77 1.519(4) . ?
C73 H73 0.9500 . ?
C73 C74 1.377(4) . ?
C74 H74 0.9500 . ?
C74 C75 1.389(4) . ?
C75 H75 0.9500 . ?
C75 C76 1.393(4) . ?
C76 C80 1.517(4) . ?
C77 H77 1.0000 . ?
C77 C78 1.529(4) . ?
C77 C79 1.523(4) . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80 1.0000 . ?
C80 C81 1.530(4) . ?
C80 C82 1.531(4) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83 0.9500 . ?
C83 C84 1.380(4) . ?
C83 N7 1.354(3) . ?
C84 H84 0.9500 . ?
C84 C85 1.376(4) . ?
C85 H85 0.9500 . ?
C85 C86 1.379(4) . ?
C86 H86 0.9500 . ?
C86 C87 1.384(4) . ?
C87 H87 0.9500 . ?
C87 N7 1.350(4) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C88 C89 1.470(10) . ?
C89 H89A 0.9900 . ?
C89 H89B 0.9900 . ?
C89 O3 1.363(8) . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?
C90 C91 1.412(12) . ?
C90 O3 1.279(9) . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
N1 Nb1 2.220(2) . ?
N2 Nb1 2.218(2) . ?
N3 Nb1 1.798(2) . ?
N4 Nb2 2.099(2) . ?
N6 Nb2 1.778(2) . ?
N7 Nb2 2.413(2) . ?
O1 Nb1 1.9385(17) . ?
O1 Nb2 1.9798(18) . ?
O2 Nb1 1.9487(17) . ?
O2 Nb2 1.9682(17) . ?
Nb1 Nb2 3.0118(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C4 115.5(2) . . ?
N1 C1 C2 124.1(2) . . ?
N1 C1 C4 120.4(2) . . ?
C1 C2 H2 115.7 . . ?
C3 C2 C1 128.6(3) . . ?
C3 C2 H2 115.7 . . ?
C2 C3 C5 115.5(2) . . ?
N2 C3 C2 124.0(2) . . ?
N2 C3 C5 120.4(2) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 119.3(2) . . ?
C11 C6 C7 121.6(2) . . ?
C11 C6 N1 118.9(2) . . ?
C6 C7 C12 123.0(2) . . ?
C8 C7 C6 117.1(3) . . ?
C8 C7 C12 120.0(2) . . ?
C7 C8 H8 119.0 . . ?
C9 C8 C7 122.0(3) . . ?
C9 C8 H8 119.0 . . ?
C8 C9 H9 120.2 . . ?
C8 C9 C10 119.7(3) . . ?
C10 C9 H9 120.2 . . ?
C9 C10 H10 119.4 . . ?
C9 C10 C11 121.3(3) . . ?
C11 C10 H10 119.4 . . ?
C6 C11 C15 122.0(2) . . ?
C10 C11 C6 118.3(3) . . ?
C10 C11 C15 119.6(3) . . ?
C7 C12 H12 108.1 . . ?
C7 C12 C13 113.2(2) . . ?
C7 C12 C14 109.5(2) . . ?
C13 C12 H12 108.1 . . ?
C14 C12 H12 108.1 . . ?
C14 C12 C13 109.8(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15 107.5 . . ?
C11 C15 C16 112.1(2) . . ?
C11 C15 C17 112.7(2) . . ?
C16 C15 H15 107.5 . . ?
C16 C15 C17 109.4(2) . . ?
C17 C15 H15 107.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N2 118.6(2) . . ?
C23 C18 C19 121.7(2) . . ?
C23 C18 N2 119.6(2) . . ?
C18 C19 C24 122.5(2) . . ?
C20 C19 C18 117.5(3) . . ?
C20 C19 C24 120.0(3) . . ?
C19 C20 H20 119.1 . . ?
C21 C20 C19 121.9(3) . . ?
C21 C20 H20 119.1 . . ?
C20 C21 H21 120.2 . . ?
C22 C21 C20 119.5(3) . . ?
C22 C21 H21 120.2 . . ?
C21 C22 H22 119.2 . . ?
C21 C22 C23 121.6(3) . . ?
C23 C22 H22 119.2 . . ?
C18 C23 C27 123.8(2) . . ?
C22 C23 C18 117.7(3) . . ?
C22 C23 C27 118.5(2) . . ?
C19 C24 H24 107.4 . . ?
C19 C24 C25 113.5(2) . . ?
C19 C24 C26 112.6(2) . . ?
C25 C24 H24 107.4 . . ?
C26 C24 H24 107.4 . . ?
C26 C24 C25 108.3(2) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27 107.5 . . ?
C23 C27 C28 112.6(2) . . ?
C23 C27 C29 111.3(2) . . ?
C28 C27 H27 107.5 . . ?
C29 C27 H27 107.5 . . ?
C29 C27 C28 110.1(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C35 C30 C31 118.6(3) . . ?
N3 C30 C31 119.6(3) . . ?
N3 C30 C35 121.7(3) . . ?
C30 C31 C36 121.4(3) . . ?
C32 C31 C30 119.5(3) . . ?
C32 C31 C36 119.1(3) . . ?
C31 C32 H32 119.3 . . ?
C33 C32 C31 121.3(3) . . ?
C33 C32 H32 119.3 . . ?
C32 C33 H33 120.3 . . ?
C34 C33 C32 119.3(3) . . ?
C34 C33 H33 120.3 . . ?
C33 C34 H34 119.1 . . ?
C33 C34 C35 121.9(3) . . ?
C35 C34 H34 119.1 . . ?
C30 C35 C39 122.0(3) . . ?
C34 C35 C30 119.3(3) . . ?
C34 C35 C39 118.6(3) . . ?
C31 C36 H36 107.3 . . ?
C31 C36 C37 110.9(2) . . ?
C31 C36 C38 113.8(2) . . ?
C37 C36 H36 107.3 . . ?
C37 C36 C38 109.9(2) . . ?
C38 C36 H36 107.3 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C39 H39 108.4 . . ?
C35 C39 C40 112.5(3) . . ?
C40 C39 H39 108.4 . . ?
C41 C39 C35 109.7(3) . . ?
C41 C39 H39 108.4 . . ?
C41 C39 C40 109.4(3) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C45 123.0(3) . . ?
C43 C42 N4 123.7(3) . . ?
N4 C42 C45 113.3(2) . . ?
C42 C43 H43 115.7 . . ?
C42 C43 C44 128.6(3) . . ?
C44 C43 H43 115.7 . . ?
C43 C44 C46 113.1(3) . . ?
N5 C44 C43 123.2(3) . . ?
N5 C44 C46 123.6(3) . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 N4 117.4(2) . . ?
C52 C47 C48 120.6(3) . . ?
C52 C47 N4 121.9(2) . . ?
C47 C48 C53 123.2(3) . . ?
C49 C48 C47 118.1(3) . . ?
C49 C48 C53 118.7(2) . . ?
C48 C49 H49 119.1 . . ?
C50 C49 C48 121.9(3) . . ?
C50 C49 H49 119.1 . . ?
C49 C50 H50 120.6 . . ?
C51 C50 C49 118.9(3) . . ?
C51 C50 H50 120.6 . . ?
C50 C51 H51 119.0 . . ?
C50 C51 C52 122.0(3) . . ?
C52 C51 H51 119.0 . . ?
C47 C52 C56 122.9(3) . . ?
C51 C52 C47 118.4(3) . . ?
C51 C52 C56 118.6(3) . . ?
C48 C53 H53 107.6 . . ?
C48 C53 C54 111.4(2) . . ?
C48 C53 C55 111.8(3) . . ?
C54 C53 H53 107.6 . . ?
C55 C53 H53 107.6 . . ?
C55 C53 C54 110.5(2) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C52 C56 H56 107.7 . . ?
C52 C56 C57 111.9(3) . . ?
C52 C56 C58 110.9(3) . . ?
C57 C56 H56 107.7 . . ?
C58 C56 H56 107.7 . . ?
C58 C56 C57 110.8(3) . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C64 C59 C60 120.2(3) . . ?
C64 C59 N5 123.5(3) . . ?
N5 C59 C60 116.1(3) . . ?
C59 C60 C65 119.2(2) . . ?
C61 C60 C59 118.6(3) . . ?
C61 C60 C65 122.1(3) . . ?
C60 C61 H61 119.4 . . ?
C62 C61 C60 121.2(3) . . ?
C62 C61 H61 119.4 . . ?
C61 C62 H62 120.0 . . ?
C61 C62 C63 120.1(3) . . ?
C63 C62 H62 120.0 . . ?
C62 C63 H63 119.3 . . ?
C62 C63 C64 121.4(3) . . ?
C64 C63 H63 119.3 . . ?
C59 C64 C68 121.9(3) . . ?
C63 C64 C59 118.5(3) . . ?
C63 C64 C68 119.6(3) . . ?
C60 C65 H65 107.3 . . ?
C66 C65 C60 110.5(2) . . ?
C66 C65 H65 107.3 . . ?
C66 C65 C67 110.5(3) . . ?
C67 C65 C60 113.7(3) . . ?
C67 C65 H65 107.3 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C65 C67 H67A 109.5 . . ?
C65 C67 H67B 109.5 . . ?
C65 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C64 C68 H68 107.9 . . ?
C64 C68 C69 111.8(3) . . ?
C64 C68 C70 110.8(3) . . ?
C69 C68 H68 107.9 . . ?
C70 C68 H68 107.9 . . ?
C70 C68 C69 110.3(3) . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C68 C70 H70A 109.5 . . ?
C68 C70 H70B 109.5 . . ?
C68 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C72 C71 C76 120.7(3) . . ?
N6 C71 C72 120.0(2) . . ?
N6 C71 C76 119.3(2) . . ?
C71 C72 C77 121.4(2) . . ?
C73 C72 C71 118.3(2) . . ?
C73 C72 C77 120.2(2) . . ?
C72 C73 H73 119.3 . . ?
C74 C73 C72 121.4(3) . . ?
C74 C73 H73 119.3 . . ?
C73 C74 H74 120.1 . . ?
C73 C74 C75 119.8(3) . . ?
C75 C74 H74 120.1 . . ?
C74 C75 H75 119.3 . . ?
C74 C75 C76 121.5(3) . . ?
C76 C75 H75 119.3 . . ?
C71 C76 C80 120.2(2) . . ?
C75 C76 C71 118.0(2) . . ?
C75 C76 C80 121.7(2) . . ?
C72 C77 H77 108.0 . . ?
C72 C77 C78 111.3(2) . . ?
C72 C77 C79 110.7(2) . . ?
C78 C77 H77 108.0 . . ?
C79 C77 H77 108.0 . . ?
C79 C77 C78 110.8(2) . . ?
C77 C78 H78A 109.5 . . ?
C77 C78 H78B 109.5 . . ?
C77 C78 H78C 109.5 . . ?
H78A C78 H78B 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C77 C79 H79A 109.5 . . ?
C77 C79 H79B 109.5 . . ?
C77 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C76 C80 H80 107.4 . . ?
C76 C80 C81 114.0(2) . . ?
C76 C80 C82 109.5(2) . . ?
C81 C80 H80 107.4 . . ?
C81 C80 C82 110.8(2) . . ?
C82 C80 H80 107.4 . . ?
C80 C81 H81A 109.5 . . ?
C80 C81 H81B 109.5 . . ?
C80 C81 H81C 109.5 . . ?
H81A C81 H81B 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C80 C82 H82A 109.5 . . ?
C80 C82 H82B 109.5 . . ?
C80 C82 H82C 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C84 C83 H83 118.8 . . ?
N7 C83 H83 118.8 . . ?
N7 C83 C84 122.5(3) . . ?
C83 C84 H84 120.1 . . ?
C85 C84 C83 119.8(3) . . ?
C85 C84 H84 120.1 . . ?
C84 C85 H85 120.7 . . ?
C84 C85 C86 118.7(3) . . ?
C86 C85 H85 120.7 . . ?
C85 C86 H86 120.6 . . ?
C85 C86 C87 118.7(3) . . ?
C87 C86 H86 120.6 . . ?
C86 C87 H87 118.3 . . ?
N7 C87 C86 123.4(3) . . ?
N7 C87 H87 118.3 . . ?
H88A C88 H88B 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C89 C88 H88A 109.5 . . ?
C89 C88 H88B 109.5 . . ?
C89 C88 H88C 109.5 . . ?
C88 C89 H89A 107.7 . . ?
C88 C89 H89B 107.7 . . ?
H89A C89 H89B 107.1 . . ?
O3 C89 C88 118.6(7) . . ?
O3 C89 H89A 107.7 . . ?
O3 C89 H89B 107.7 . . ?
H90A C90 H90B 105.8 . . ?
C91 C90 H90A 104.8 . . ?
C91 C90 H90B 104.8 . . ?
O3 C90 H90A 104.8 . . ?
O3 C90 H90B 104.8 . . ?
O3 C90 C91 129.8(10) . . ?
C90 C91 H91A 109.5 . . ?
C90 C91 H91B 109.5 . . ?
C90 C91 H91C 109.5 . . ?
H91A C91 H91B 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C1 N1 C6 114.6(2) . . ?
C1 N1 Nb1 122.92(16) . . ?
C6 N1 Nb1 121.34(16) . . ?
C3 N2 C18 114.8(2) . . ?
C3 N2 Nb1 122.80(16) . . ?
C18 N2 Nb1 121.29(16) . . ?
C30 N3 Nb1 173.33(18) . . ?
C42 N4 C47 114.8(2) . . ?
C42 N4 Nb2 115.23(18) . . ?
C47 N4 Nb2 129.52(17) . . ?
C44 N5 C59 122.9(3) . . ?
C71 N6 Nb2 170.3(2) . . ?
C83 N7 Nb2 119.11(18) . . ?
C87 N7 C83 116.9(2) . . ?
C87 N7 Nb2 124.04(17) . . ?
Nb1 O1 Nb2 100.46(8) . . ?
Nb1 O2 Nb2 100.51(7) . . ?
C90 O3 C89 130.4(8) . . ?
N1 Nb1 Nb2 123.55(6) . . ?
N2 Nb1 N1 82.26(8) . . ?
N2 Nb1 Nb2 116.48(6) . . ?
N3 Nb1 N1 101.14(9) . . ?
N3 Nb1 N2 105.86(9) . . ?
N3 Nb1 O1 111.84(9) . . ?
N3 Nb1 O2 112.77(9) . . ?
N3 Nb1 Nb2 120.40(8) . . ?
O1 Nb1 N1 146.75(8) . . ?
O1 Nb1 N2 84.73(8) . . ?
O1 Nb1 O2 80.24(7) . . ?
O1 Nb1 Nb2 40.27(5) . . ?
O2 Nb1 N1 91.18(7) . . ?
O2 Nb1 N2 141.36(8) . . ?
O2 Nb1 Nb2 39.98(5) . . ?
N4 Nb2 N7 88.45(8) . . ?
N4 Nb2 Nb1 130.03(6) . . ?
N6 Nb2 N4 101.70(10) . . ?
N6 Nb2 N7 99.28(8) . . ?
N6 Nb2 O1 111.48(9) . . ?
N6 Nb2 O2 108.77(8) . . ?
N6 Nb2 Nb1 117.05(8) . . ?
N7 Nb2 Nb1 113.24(5) . . ?
O1 Nb2 N4 145.30(8) . . ?
O1 Nb2 N7 76.75(7) . . ?
O1 Nb2 Nb1 39.27(5) . . ?
O2 Nb2 N4 100.38(8) . . ?
O2 Nb2 N7 147.97(7) . . ?
O2 Nb2 O1 78.77(7) . . ?
O2 Nb2 Nb1 39.51(5) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 372.9 35.1 ?
2 0.122 0.569 0.848 8.5 0.0 ?
3 0.254 0.034 0.394 58.5 0.9 ?
4 0.246 0.534 0.106 58.5 0.9 ?
5 0.500 0.500 0.500 372.9 35.1 ?
6 0.378 0.069 0.652 8.5 0.0 ?
7 0.622 0.931 0.348 8.5 0.0 ?
8 0.746 -0.034 0.606 58.5 0.9 ?
9 0.754 0.466 0.894 58.5 0.9 ?
10 0.878 0.431 0.152 8.5 0.0 ?


_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Diethyl ether'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
